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  • 1995-1999  (5.358)
  • 1980-1984  (8.927)
  • Cell & Developmental Biology  (6.901)
  • Analytical Chemistry and Spectroscopy  (6.605)
  • Ultrastructure
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  • 1
    Digitale Medien
    Digitale Medien
    Springer
    Sexual plant reproduction 12 (1999), S. 99-109 
    ISSN: 1432-2145
    Schlagwort(e): Key words Arabidopsis thaliana ; Megasporogenesis ; Meiosis ; Ultrastructure ; Cellular polarity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract  In this study, megasporogenesis of the plant model Arabidopsis thaliana was investigated by electron microscopy for the first time. The data described here could constitute a reference for future investigations of Arabidopsis mutants. During the beginning of meiosis the megaspore mother cell shows a polarity created by unequal distribution of organelles in the cytoplasm. Plastids accumulate in the chalazal region and long parallel saccules of endoplasmic reticulum, small vacuoles and some dictyosomes are found in the micropylar region. Plasmodesmata are abundant in the chalazal cell wall. The nucleus is almost centrally localized and contains a prominent excentric nucleolus and numerous typical synaptonemal complexes. After the second division of meiosis the four megaspores are separated by thin cell walls crossed by numerous plasmodesmata and do not show significant cellular organization. The young functional megaspore is characterized by a large nucleus and a large granular nucleolus. The cytoplasm is very electron dense due to the abundance of free ribosomes and contains the following randomly distributed organelles: mitochondria, a few short saccules of endoplasmic reticulum, dictyosomes and undifferentiated plastids. However, there is no apparent polarity, except for the distribution of some small vacuoles which are more abundant in the micropylar region of the cell. The degenerating megaspores are extremely electron dense and do not show any substructure.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Virchows Archiv 435 (1999), S. 13-19 
    ISSN: 1432-2307
    Schlagwort(e): Key words Inflammation of the lung ; Biopsy ; Ultrastructure ; Laser therapy
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract  Examination of 127 biopsy specimens from 45 patients with inflammatory lung diseases showed changes consistent with increased permeability of the capillary endothelial cells as an initial stage in the development of the inflammatory reaction. Associated interstitial oedema, deformation of the interalveolar septa, and structural disorganization of alveolar epithelium cells occur, and local microcirculatory problems result in tissue hypoxia and fibrosis. The ultimate morphological picture is determined largely by the intensity of repair. Laser biostimulation minimizes the inflammation and stabilizes fibroplastic process.
    Materialart: Digitale Medien
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Virchows Archiv 435 (1999), S. 58-61 
    ISSN: 1432-2307
    Schlagwort(e): Key words Capillary basement membrane ; Inflammatory myopathy ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract  The capillary basement membranes from 16 skeletal muscle biopsies from patients with a clinical and histological diagnosis of inflammatory myopathy and from six controls were analysed ultrastructurally and morphometrically. Resin sections from 244 endomysial capillaries were examined by light microscope, and the results were correlated with findings seen in electron micrographs of these capillaries. The ultrastructural morphometric measurements and the statistical analysis showed that the capillary basement membrane was thick and multilaminated in 87% specimens affected by inflammatory myopathy. No thick or multilaminated basement membrane was observed in controls. In inflammatory myopathy the endomysial space next to the capillaries contained an increased amount of collagen fibrils and showed signs of a chronic reparative process. It is suggested that the thick multilaminated basement membrane in inflammatory myopathy represents an advanced stage of vascular regeneration.
    Materialart: Digitale Medien
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  • 4
    ISSN: 1432-0533
    Schlagwort(e): Key words Polyglucosan body ; Periodic ; acid-Schiff-positive granules ; Mouse brain ; Immunohistochemistry ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Periodic acid-Schiff-positive granules (PGs) appear in the mouse brains in relation to advancing age. The exact location and pathophysiological significance of PGs, however, are not fully understood. The incidence, staining properties, and topographical distributions of PGs in the brains of 17 AKR mice ranging in age from 7 to 18 months were examined histochemically and immunohistochemically using antibody KM279 raised against a polyglucosan. In addition, to define the precise site of PG formation, we investigated the brains of 4 AKR mice of 24 months of age using conventional and immunoelectron microscopy. PGs were seen in all mice examined and the levels were increased with age. The PGs were located predominantly in the hippocampus and, to a lesser extent, in the cerebellum and olfactory bulb. Immunohistochemically, PGs in the hippocampus and cerebellum were labeled uniformly with KM279. On immunoelectron microscopy with this monoclonal antibody, the fibrillar or membranous structures corresponding to PGs seen using light microscopy were labeled specifically with gold particles. With conventional electron microscopy, fibrillar or membranous structures were seen along with synaptic vesicles and dense-core granules. Moreover, around the cells containing PGs, a few synaptic junctions with neighboring cells were observed, indicating that the cells contributing to formation of PGs were neuronal cells. The positive immunoreactivity of AKR mouse PGs for the antibody KM279 suggests that the PGs and similar structures in other species may share a common antigenicity. Thus, it is assumed that PGs in AKR mice might result from some abnormalities in glucose metabolism.
    Materialart: Digitale Medien
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  • 5
    ISSN: 1432-0533
    Schlagwort(e): Key words Amyloid precursor protein ; immunoreactivity ; Axonal injury ; Microwave antigen retrieval ; Traumatic brain injury ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Antibodies to the amyloid precursor proteins (APP) have become routine markers for detecting traumatically induced axonal injury (AI) in animals and man. Unfortunately, the techniques used to visualize these proteins are not compatible with routine electron microscopic (EM) analysis. In the current communication, we describe a method for the ultrastructural visualization of antibodies to APP and, using this method, we identify a previously unrecognized population of traumatically injured axons. Rats were subjected to an impact acceleration traumatic brain injury and allowed to survive 30 min to 3 h postinjury. The animals were then perfused, their brains sectioned on a vibratome and the sections prepared for immunocytochemistry using a computer-controlled microwave capable of temperature regulation. The use of temperature-controlled microwave energy unmasked APP antigenic epitopes without sacrificing ultrastructural detail. The APP antibody was found in two distinct populations of reactive axons that differed in size, morphology, location, and temporal progression. Comparable to previous descriptions, one population showed traumatically related reactive changes that led to swelling and disconnection. The other population, however, revealed unanticipated changes reflected in nodal and paranodal swelling of small continuous fibers that showed no evidence of disconnection during the time periods assessed. These studies provide new insight into the complexity of the pathobiology of AI, while describing a novel approach for enhancing APP immunoreactivity at the EM level.
    Materialart: Digitale Medien
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  • 6
    ISSN: 1432-0568
    Schlagwort(e): Key words Intrinsic laryngeal motoneurons ; Cholera toxin HRP ; Ultrastructure ; Swallowing ; Respiration
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract  The laryngeal motoneurons innervating the cricothyroid muscle (CT) are located in the semicompact formation just ventral to the rostral part of the compact formation of the nucleus ambiguus. The motoneurons innervating the posterior cricoarytenoid muscle (PCA) are located in the loose formation. We retrogradely labeled the CT and the PCA motoneurons using cholera toxin subunit B-conjugated horseradish peroxidase, and determined the ultrastructure and synaptic organization of these neurons. The CT and the PCA motoneurons had the appearance of α-motoneurons, i.e., large, oval or polygonal cells containing well-developed organelles and a prominent spherical nucleus. Two kinds of neurons were recognized among the PCA motoneurons. The one (PCA-A) was significantly smaller than the other (PCA-B). The average number of axosomatic terminals in a section was significantly largest in the PCA-B (56.6), smaller in the PCA-A (36.0), and smallest in the CT (32.3) neurons. Most of the axosomatic terminals (64.7%) contained pleomorphic vesicles and made symmetric synaptic contacts (Gray’s type II) with the PCA-A neurons, while more than 60% contained round vesicles with asymmetric synaptic contacts (Gray’s type I) in the CT (69.5%) and the PCA-B (60.6%) neurons. A few terminals associated with subsurface cisterns were present on all laryngeal motoneurons. These results indicated that the CT motoneurons may receive mostly excitatory terminals, whereas the PCA muscle may be regulated by neurons having many inhibitory terminals, and neurons having many excitatory terminals.
    Materialart: Digitale Medien
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  • 7
    ISSN: 1432-0533
    Schlagwort(e): Key words Amyotrophic lateral sclerosis ; Bunina body ; Guam ; Immunohistochemistry ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract An investigation of Bunina bodies is important when studying the pathoetiology and pathomechanisms involved in amyotrophic lateral sclerosis (ALS). It may serve as a clue essential for the study of the pathogenesis of Guamanian amyotrophic lateral sclerosis (ALS-G), and it may provide a means of answering the question of whether ALS-G is the same disease as classical ALS or a different entity. In ALS-G, however, no precise histochemical, immunohistochemical, or detailed ultrastructural examination has been published to date. To elucidate the pathological differences/similarities of Bunina bodies between classical ALS and ALS-G, we performed histochemical, immunohistochemical, topographic and ultrastructural examinations. Histochemically, hematoxylin and eosin, Masson’s trichrome, methylgreen-pyronin, phosphotungstic acid-hematoxylin, Klüver-Barrera, Bodian and periodic acid-Schiff staining were utilized. Immunohistochemical examination was performed using antibodies for cystatin C, ubiquitin, Tau-2, Cu/Zn superoxide dismutase, phosphorylated neurofilament and glial fibrillary acidic protein. Histochemical findings were consistent with those previously described for classical ALS. The immunohistochemical study showed that in ALS-G Bunina bodies were intensely labeled by an anti-cystatin C antibody. Topographic examination demonstrated that Bunina bodies were distributed in the spinal anterior horns and Clarke’s column in the spinal cord. Ultrastructurally, Bunina bodies were composed of electron-dense amorphous/ granular material accompanied by vesicular structures and neurofilaments. The results of the present study have revealed that the pathological features of Bunina bodies in ALS-G are identical to those seen in classical ALS. These findings strongly suggest that a similar degenerative process occurs in the spinal anterior horn cells in both ALS-G and classical ALS.
    Materialart: Digitale Medien
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  • 8
    ISSN: 1432-0533
    Schlagwort(e): Key words Ischemia ; Protein synthesis ; Translation ; Ultrastructure ; Hippocampus
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract During post-ischemic brain reperfusion there is a substantial reduction of protein synthesis in selectively vulnerable neurons. Normal protein synthesis requires a functional translation initiation complex, a key element of which is eukaryotic initiation factor 2 (eIF2), which in a complex with GTP introduces the met-tRNAi. Phosphorylation of Ser51 on the α subunit of eIF2 [eIF2α(P)] generates a competitive inhibitor of eIF2B, thereby preventing the replenishment of GTP onto eIF2, thus blocking translation initiation. It has been shown that the conditional expression of an eIF2α mutant (Asp substituted for Ser51) imitating the negative charge of Ser51 (P) induces apoptosis. During the first 10 min of post-ischemic reperfusion, there is an approximately 20-fold increase in eIF2α(P) seen in the cytoplasm of CA1 hippocampal neurons, and, by 1 h, there is also accumulation of eIF2α(P) in the nucleus. We utilized post-embedding electron microscopical immunogold methods to examine the localization of eIF2α(P) during reperfusion. Immunogold particles (10 nm) were concentrated chiefly along the rough endoplasmic reticulum and in association with the membranes of the nuclear envelope in CA1 neurons. Aggregations of gold particles in the nucleus were concentrated: (1) within and around the nucleolus, (2) associated to strands of heterochromatin, and (3) along putative nuclear filaments. The presence of eIF2α(P) in the nucleolus probably reflects its association with nascent ribosomal subunits. The β-subunit of eIF2 has a zinc finger and polylysine blocks analogous to those on other proteins that affect transcription. The association of eIF2α(P) with chromatin may have important implications for transcription.
    Materialart: Digitale Medien
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  • 9
    Digitale Medien
    Digitale Medien
    Springer
    Anatomy and embryology 199 (1999), S. 407-418 
    ISSN: 1432-0568
    Schlagwort(e): Key words Placenta ; Vascular wall ; Smooth muscle cell ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract  The vascular wall structure in the human full-term placental villi of normal pregnancy was studied by means of light and electron microscopy with an improved technique of perfusion fixation and tissue preparation. We observed 81 sections of stem villi that showed cross-sectional profiles of paired vessels in their center. Both vascular walls contained a large amount of extracellular matrix and no elastic lamina between smooth muscle cells of the media, making identification of the artery and the vein quite difficult at first sight. We then noted that the density of the smooth muscle cell population was always considerably higher in one than the other, and identified the former as artery and the latter as vein on the basis of their connection with larger arteries and veins running on the chorionic plate. Between the paired vessels, the artery had a smaller caliber than the vein, and the ratio of venous to arterial caliber was distributed from 1.0 to 2.5. The thickness of media was usually thicker in the vein than in the artery. Clusters of elastic fibers were found occasionally in the media of arteries and veins, and basement membrane-like materials were associated frequently with the elastic fibers and were distributed widely in the media as well as in the adventitia. In the veins, the smooth muscle cells of the most superficial part of the media contained well-developed rough endoplasmic reticulum and Golgi apparatus, indicating differentiation to secrete extracellular matrices. The present study revealed the difference of wall structure between arteries and veins in the placental stem villi for the first time at the ultrastructural level, and suggested differentiation of venous smooth muscle cells, possibly by some influence from the luminal side.
    Materialart: Digitale Medien
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  • 10
    Digitale Medien
    Digitale Medien
    Springer
    Anatomy and embryology 200 (1999), S. 81-90 
    ISSN: 1432-0568
    Schlagwort(e): Key words Elastic fibre system ; Microfibrils ; Collagen type IV ; Ultrastructure ; Immunocytochemistry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract  This study deals with the examination of the elastic fibre system as well as collagen fibrils and collagen type IV in the amnion of the human chorionic plate of uncomplicated pregnancies at term. In organs other than placenta, the elastic fibre system comprises elastic fibres, elaunin and oxytalan microfibrils. The investigation was performed by light and electron microscopy and immunocytochemistry. Abundant oxytalan fibres were present in all amnionic layers, while no elastic fibres were found. Oxytalan microfibrils formed a broad subepithelial layer and were intermingled with collagen fibrils in the subjacent compact layer and in the amnionic mesoderm. Light microscopically, bunches containing orcein-stained oxytalan and collagen-type-IV-immunostained microfibrils were seen rising from the amnionic mesoderm perpendicularly towards the epithelial layer, where they obviously inserted. It can be assumed that the subepithelial microfibrillar layer and the following compact layer form an anchoring zone between the amnionic mesoderm and the epithelium that may contribute to the maintenance of strength. The ultrastructure of the bunches clearly showed collagen fibrils mixed with oxytalan microfibrils. No collagen type I-immunostaining was found in the bunches. After pretreatment of cryostat sections with elastase, oxytalan-orcein-staining was absent, but collagen type IV-immunoreactivity was not altered. Furthermore, after oxytalan-orcein-staining resp. anti-collagen type IV incubation, all positive fibres revealed an identical morphological pattern. We propose that oxytalan and collagen type IV may represent further members of the microfibril complex.
    Materialart: Digitale Medien
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  • 11
    Digitale Medien
    Digitale Medien
    Springer
    Acta neuropathologica 97 (1999), S. 509-514 
    ISSN: 1432-0533
    Schlagwort(e): Key words Hereditary inclusion body myopathy ; Desmin storage myopathy ; Ultrastructure ; Immmunocytochemistry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract We report two adult familial cases of inclusion body myopathy (IBM) with desmin storage in skeletal muscle. Clinically, both patients presented late-onset, progressive, symmetrical, both proximal and distal muscle weakness. Muscle biopsy findings were identical in both cases and consisted of marked variability in fiber size, increased number of central nuclei and vacuolation involving 10% of fibers. Single or multiple vacuoles were located subsarcolemmally or in the center, and were rimmed by basophilic material. At the ultrastructural level, tubulofilamentous nuclear and cytoplasmic inclusions of 16–21 nm in diameter were frequently observed. In addition, large subsarcolemmal and central deposits composed of electron-dense granular material were present in many fibers. Immunocytochemistry revealed staining for desmin, vimentin and ubiquitin within both inclusions and vacuolated fibers. Possible structural and functional associations between these two types of muscle changes remain unclear. They may either represent two coexistent disease processes or merely reflect an abnormal form of muscle fiber degradation, with unidentifiable specificity.
    Materialart: Digitale Medien
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  • 12
    ISSN: 1432-041X
    Schlagwort(e): Key words Imaginal disc ; Axonal trajectories ; Ultrastructure ; Chaoborus (Insecta ; Diptera)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract  In one of his classical studies on insect metamorphosis, Weismann compared the imaginal anlagen of the ancestral phantom midge, Chaoborus, with those of advanced brachycerans. We have expanded his findings on the relationships between larval and imaginal organs using electron microscopy and cobalt backfilling of the antenna and leg anlagen and the axonal trajectories of corresponding larval sensilla. We show that both primordia are confluent with the larval antennae and ”leg” sensilla (an ancestral Keilin organ), respectively. These fully developed larval organs represent the distal tips of the imaginal anlagen rather than separate cell clusters. The axons of the larval antenna and leg sensilla project across the corresponding anlagen to their target neuromeres within the central nervous system (CNS). Within the discs, nerves composed of these larval axons, developing afferent fibres and efferences ascending from the CNS are found. Both the structure of the primordia and the axonal trajectories thus relate the situation found in advanced brachycerans with that seen in more ancestral insects. In addition, the larval antennae, legs, wings and even the eyes possess very similar afferent pioneer trajectories supporting the idea that the described pattern is generally used in the ontogeny of sensory systems.
    Materialart: Digitale Medien
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  • 13
    ISSN: 1432-072X
    Schlagwort(e): Key wordsClostridium xylanolyticum ; Cinnamic acid ; Esterase ; Lignocellulose ; Sporogenesis ; Ultrastructure ; Cell envelope
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Microorganisms that hydrolyse the ester linkages between phenolic acids and polysaccharides in plant cell walls are potential sources of enzymes for the degradation of lignocellulosic waste. An anaerobic, mesophilic, spore-forming, xylanolytic bacterium with high hydroxy cinnamic acid esterase activity was isolated from the gut of the grass-eating termite Tumilitermes pastinator. The bacterium was motile and rod-shaped, stained gram-positive, had an eight-layered cell envelope, and formed endospores. Phylogenetic analysis based on 16S rRNA indicated that the bacterium is closely related to Clostridium xylanolyticum and is grouped with polysaccharolytic strains of clostridia. A wide range of carbohydrates were fermented, and growth was stimulated by either xylan or cellobiose as substrates. The bacterium hydrolysed and then hydrogenated the hydroxy cinnamic acids (ferulic and p-coumaric acids), which are esterified to arabinoxylan in plant cell walls. Three cytoplasmic enzymes with hydroxy cinnamic acid esterase activity were identified using non-denaturing gel electrophoresis. This bacterium possesses an unusual multilayered cell envelope in which both leaflets of the cytoplasmic membrane, the peptidoglycan layer and the S layer are clearly discernible. The fate of all these components was easily followed throughout the endospore formation process. The peptidoglycan component persisted during the entire morphogenesis. It was seen to enter the septum and to pass with the engulfing membranes to surround the prespore. It eventually expanded to form the cortex, verification for the peptidoglycan origin of the cortex. Sporogenic vesicles, which are derived from the cell wall peptidoglycan, were associated with the engulfment process. Spore coat fragments appeared early, in stage II, though spore coat formation was not complete until after cortex formation.
    Materialart: Digitale Medien
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  • 14
    Digitale Medien
    Digitale Medien
    Springer
    Experimental brain research 124 (1999), S. 89-99 
    ISSN: 1432-1106
    Schlagwort(e): Key words Microglial culture ; Brain macrophages ; Isolectin ; Ultrastructure ; Intracellular pathway
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract  The present study examined the lectin labeling of diverse morphological forms of microglia in culture. Similar to amoeboid microglial cells in vivo, polymorphic microglia showed lectin labeling at their plasma membranes, as well as in a few cytoplasmic vesicles and vacuoles. This labeling pattern was observed in cultured microglia incubated with isolectin at 4°C for 30 min. Five minutes after the temperature was raised to 37°C, the surface lectin receptors appeared to be internalized, as shown by the occurrence of many subsurface lectin-labeled vesicles, vacuoles and tubule-like structures. With longer incubation (up to 1–2 h at 37°C), many lysosomes and a few trans-Golgi saccules and associated lysosome-like structures became labeled. Concomitant with these changes was a reduction of lectin labeling at the plasma, with labeling having vanished in most of the cells after 1–2 h of incubation. By 24 h, only a few cells retained surface lectin labeling. It appears, therefore, that irrespective of morphology, lectin labeling (including its intracellular pathway) of microglia in culture parallels that of amoeboid microglia in vivo. This would offer a useful model for the study of lectin turnover in microglia and help to explain the roles of such receptors in microglial differentiation and function.
    Materialart: Digitale Medien
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  • 15
    ISSN: 1432-069X
    Schlagwort(e): Key words p75 nerve growth factor receptor ; (p75 NGFr) ; Immunoreactivity ; Ultrastructure ; Prurigo nodularis ; Nerve fiber
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Prurigo nodularis is an inflammatory skin disease characterized by neurohyperplasia. Neurotrophins and their receptors play a critical role in nerve growth, differentiation, maturation and maintenance, including cutaneous nerve fiber growth and innervation. They may also be responsible for events related to the growth and differentiation control of keratinocytes. To explore the exact distribution of the p75 low-affinity nerve growth factor receptor (p75 NGFr) in the cutaneous nerve components, p75 NGFr immunofluorescence as well as ultrastructural immunohistochemical studies were performed on prurigo nodularis lesional skin and normal human skin samples. The immunofluorescence results revealed that nerve fibers and bundles were increased in number and size in lesional upper dermis with stronger p75 NGFr immunoreactivity than in the corresponding normal tissue. At the ultrastructural level, a lot of nerve fibers clustered together in the prurigo nodularis dermal tissue. The axons were enlarged and branched, but the axons themselves seldom showed any NGFr immunoreactivity. The Schwann cell bodies were extended and irregularly shaped, and tended to separate into many branches enveloping the axons. The Schwann cell membrane showed strong p75 NGFr immunoreactivity. The perineurium cells also revealed strong p75 NGFr immunoreactivity. The Schwann cells inside the perineurium were less p75 NGFr-immunoreactive than those outside the perineurium. The membrane of certain basal keratinocytes showed NGFr immunoreactivity as well. The present results indicate that overexpression of p75 NGFr in Schwann cells and perineurium cells could contribute to the neurohyperplasia in prurigo nodularis.
    Materialart: Digitale Medien
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  • 16
    Digitale Medien
    Digitale Medien
    Springer
    Urological research 27 (1999), S. 454-461 
    ISSN: 1434-0879
    Schlagwort(e): Key words Cold-restraint stress ; Urinary bladder ; Interstitial cystitis ; Mast cell ; Urothelium ; Ultrastructure ; Ruthenium red ; Flow cytometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Stress is associated with many diseases of unknown aetiology. This study demonstrates the effects of cold-restraint stress on the morphology of the urinary bladder. Additionally, it compares the results obtained with the morphology of the interstitial cystitis. The animals were subjected to three hours of cold-restraint stress and then starved for 48 h. The morphology and histochemistry of the urinary bladder was investigated with light and electron microscopy. The proliferative activity was analysed via flow cytometry. Increased and degranulated mast cells in the mucosa, leucocyte infiltration in the lamina propria, vacuole formation in the urothelial cells, loose tight junction, dilated intercellular spaces and altered proliferative activity were observed in the stress group when compared with the control. The increase in the number of mast cells and especially degranulated mast cells and vacuole formation and the loose tight junction of the urothelium correlated with the histopathological findings of interstitial cystitis.
    Materialart: Digitale Medien
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  • 17
    Digitale Medien
    Digitale Medien
    Springer
    Protoplasma 206 (1999), S. 57-72 
    ISSN: 1615-6102
    Schlagwort(e): Anatomy ; Floral nectary ; Modified stomata ; Phloem ; Pisum sativum ; Stereology ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary The floral nectary ofPisum sativum L. is situated on the receptacle at the base of the gynoecium. The gland receives phloem alone which departed the vascular bundles supplying the staminal column. Throughout the nectary, only the companion cells of the phloem exhibited wall ingrowths typical of transfer cells. Modified stomata on the nectary surface served as exits for nectar, but stomatal pores developed well before the commencement of secretion. Furthermore, stomatal pores on the nectary usually closed by occlusion, not by guard-cell movements. Pore occlusion was detected most frequently in post-secretory and secretory glands, and less commonly in pre-secretory nectaries. A quantitative stereological study revealed few changes in nectary fine structure between buds, flowers secreting nectar, and post-secretory flowers. Dissolution of abundant starch grains in plastids of subepidermal secretory cells when secretion commenced suggests that starch is a precursor of nectar carbohydrate production. Throughout nectary development, mitochondria were consistently the most plentiful organelle in both epidermal and subepidermal cells, and in addition to the relative paucity of dictyosomes, endoplasmic reticulum, and their associated vesicles, the evidence suggests that floral nectar secretion inP. sativum is an energy-requiring (eccrine) process, rather that granulocrine.
    Materialart: Digitale Medien
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  • 18
    ISSN: 1615-6102
    Schlagwort(e): Cumulus oophorus ; Ovarian follicle ; Fertilization ; Ultrastructure ; Immunocytochemistry ; Human
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary The fine structure of the human cumulus oophorus has been reviewed on the basis of scanning and transmission electron microscopic observations as well as of immunofluorescence data. Tissues sampled from preovulatory ovarian follicles and cumulus-enclosed oocytes and fertilized eggs (collected from the oviduct or obtained during in vitro fertilization procedures) have been evaluated from a microtopographic and morphodynamic point of view in order to better clarify the possible role of this population of cells. In particular, the following aspects have been studied and discussed: the presence of multiple close contacts (modulated by the interposition of the zona pellucida) between the oocyte surface and the long microvillous evaginations projecting from the inner aspect of corona cells surface (through these structures the intraovarian cumulus oophorus may control oocyte growth and metabolism up until the time of ovulation); the occurrence of different subpopulations of cells (steroid-synthetic cells, cells producing adhesive proteins, leukocytes, macrophages) in the postovulatory, extraovarian cumulus oophorus surrounding oocytes, zygotes and early developing embryos. All these elements found in the cumulus mass may positively act, through their paracrine activities, on the chemical composition of the microenvironment in which fertilization occurs.
    Materialart: Digitale Medien
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  • 19
    ISSN: 1615-2573
    Schlagwort(e): Endomyocardial biopsy ; Dilated cardiomyopathy ; Children ; Ultrastructure ; Basal lamina layering of capillary
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Summary We analyzed the electron-microscopic features of endomyocardial biopsy from pediatric patients with dilated cardiomyopathy (DCM). The specimens examined were taken from the right ventricle of ten patients aged from 2 to 15 years (mean 9.7 years). Biopsy specimens from eight patients with congenital heart disease (tetralogy of Fallot), aged from 3 to 12 (mean 7.3 years), and ten adult patients with DCM, aged from 32 to 60 (mean 45 years), were also examined. Patients considered to have endocardial fibroelastosis, arrhythmogenic right ventricular cardiomyopathy, specific cardiomyopathy, or coronary heart disease were excluded from this study. Specimens from pediatric patients with DCM showed various degrees of ultrastructural abnormalities of myocytes, including myofibrillar fragmentation, mitochondrial abnormalities, and intracellular edema. The ultrastructurally determined contractility failure index based on the severity of myocardial degeneration at the electronmicroscopic level was 4.9 ± 1.1. This value was significantly higher than that in patients with tetralogy of Fallot (0.9 ± 0.6,P 〈 0.001) but was not significantly different from that in adult patients with DCM (6.1 ± 2.6). The index of pediatric patients with DCM who died within 3 years was high (6.0 ± 0.8). Basal lamina layering of a capillary (BLL) in the myocardium was revealed in 1 of the 10 (10%) pediatric patients with DCM and in 6 of the 10 (60%) adult patients with DCM (P 〈 0.05). No BLL was noted in the patients with tetralogy of Fallot. These findings may be related to the pathogenesis of DCM in children and adults.
    Materialart: Digitale Medien
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  • 20
    ISSN: 1432-0878
    Schlagwort(e): Key words Neuromelanin ; Neuron ; Peroxidase ; Oxygen metabolism ; High-definition light microscopy ; Electron microscopy ; Ultrastructure ; Cytochemistry ; Substantia nigra ; Lumbricusterrestris (Annelida)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract Histochemical examination of 1-μm tissue sections from the dorsal nerve plexus of the earthworm, Lumbricus terrestris, reveals multiple brown intraneuronal granules. These granules contain material morphologically and histochemically consistent with neuromelanin. When viewed with transmission electron microscopy, these were seen as single membrane-enclosed biphasic granules with diameters of 370–730 nm. Exposure of L. terrestris to high-level environmental oxygen resulted in an increase in the number of neuromelanin-like pigment granules within the neurons of the circular muscle layer. As measured by ortho-phenylenediamine hydrochloride, the endogenous peroxidase activity of extracts from worms incubated in high-level environmental oxygen was 51% more than controls. The endogenous peroxidase activity was localized in situ with 3,3-diaminobenzidine (DAB) and was found to increase in and around the neuromelanin-like pigment-containing neurons within the circular muscle layer. These studies suggest that the nerve net of L. terrestris may serve as a model to study the role of neuromelanin production in oxidative stress and its relationship to endogenous peroxidases.
    Materialart: Digitale Medien
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  • 21
    Digitale Medien
    Digitale Medien
    Springer
    Parasitology research 85 (1999), S. 999-1006 
    ISSN: 1432-1955
    Schlagwort(e): Key wordsEchinococcus granulosus ; Praziquantel ; Metacestode ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The efficacy of praziquantel against the metacestode of Echinococcus granulosus was studied by means of in vitro incubations or in vivo experiments. The results of in vitro incubations indicated that the effectiveness of praziquantel was higher when the parasite material comprised cysts from cyst masses than in the case of intact cysts that retained their adventitial layer. Ultrastructural alterations in the germinal layer of collapsed cysts incubated in vitro were detected. The results obtained in mice after 4 months of treatment demonstrated no significant difference between the control and treated groups with regard to the number and wet weight of developed cysts. However, ultrastructural alterations were detected in the cyst tissue that were similar to those described in the in vitro experiment. In contrast, the effect of chemoprophylaxis on the number and the wet weight of developed cysts was extremely significant as compared with the control value, the efficacy being 99.41% and 98.32%, respectively. Moreover, ultrastructural observations of the cyst tissue revealed loss of its integrity, and no intact cyton was observed in the germinal layer of the developed cyst.
    Materialart: Digitale Medien
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  • 22
    ISSN: 1432-1955
    Schlagwort(e): Key words Monogenea ; Capsalidae ; Benedenia rohdei ; B. lutjani ; Ectoparasites ; Lutjanus carponotatus ; Glands ; Ultrastructure ; Adhesion ; Attachment
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The anterior adhesive areas of Benedenia rohdei from the gills and B. lutjani from the pelvic fins of Lutjanuscarponotatus at Heron Island, Australia, were studied using scanning and transmission electron microscopy. All specimens were fixed when detached from host tissue. Both monogenean species have two disc-like anteroventral attachment organs, each of which has an anterolateral adhesive area divided into three adjacent zones by tegument from the ventral surface of the attachment organ. A rod-shaped secretion and a smaller, roughly spherical secretion are associated with the anterior adhesive areas in both species; a third type of secretion occurs anteriorly but outside these adhesive areas. The electron-dense spherical secretory bodies released onto the anterior adhesive zones in these Benedenia spp. are of a single type and differ ultrastructurally from those previously reported in monogeneans living on teleost hosts. A correlation, therefore, between secretion morphology and host type is not supported. No relationship was found between parasite microhabitat and secretion morphology.
    Materialart: Digitale Medien
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  • 23
    Digitale Medien
    Digitale Medien
    Springer
    Journal of comparative physiology 169 (1999), S. 351-359 
    ISSN: 1432-136X
    Schlagwort(e): Key words Freeze tolerance ; Sciatic nerve ; Cryoinjury ; Dehydration ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract We investigated function and ultrastructure of sciatic nerves isolated from wood frogs (Rana sylvatica) endemic to the Northwest Territories, Canada, following freezing at −2.5 °C, −5.0 °C, or −7.5 °C. All frogs frozen at −2.5 °C, and most frogs (71%) frozen at −5.0 °C, recovered within 14 h after thawing began; however, frogs did not survive exposure to −7.5 °C. Sciatic nerves isolated from frogs frozen at −7.5 °C were refractory to electrical stimulation, whereas those obtained from frogs surviving exposure to −2.5 °C or −5.0 °C generally exhibited normal characteristics of compound action potentials. Frogs responded to freezing by mobilizing hepatic glycogen reserves to synthesize the cryoprotectant glucose, which increased 20-fold in the liver and 40-fold in the blood. Ultrastructural analyses of nerves harvested from frogs in each treatment group revealed that freezing at −2.5 °C or −5.0 °C had little or no effect on tissue and cellular organization, but that (lethal) exposure to −7.5 °C resulted in marked shrinkage of the axon, degeneration of mitochondria within the axoplasm, and extensive delamination of myelin sheaths of the surrounding Schwann cells.
    Materialart: Digitale Medien
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  • 24
    ISSN: 1861-387X
    Schlagwort(e): Meningioma ; Intranuclear inclusion ; Immunohistochemistry ; Ultrastructure ; Intermediate filament
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract We describe a case of meningothelial meningioma with a large number of intranuclear inclusions. Morphologically, these are divided into cytoplasmic inclusions and nuclear vacuoles. The cytoplasmic inclusion has a limiting membrane with cell organelles and filaments. Inclusions of this type are generally eosinophilic, like the cytoplasm. However, there are many inclusions that are more eosinophilic than the cytoplasm or that have a ground-glass appearance. Some of them may contain fine or coarse granules. On the other hand, the nuclear vacuole lacks a limiting membrane and appears empty. In most of the inclusions of this type, there is a faintly basophilic substance in the margin. Generally, the cytoplasmic inclusions are as immunopositive as cytoplasm with vimentin, but some of these cytoplasmic inclusions are more reactive. Under the electron microscope, abnormal aggregation of intermediate filaments is recognized in the cytoplasmic inclusions. It is considered that a strong reaction of cytoplasmic inclusions with vimentin immunostaining is due to abnormal aggregation of intermediate filaments. The present study distinctly demonstrates abnormal localization of intermediate filaments in the cytoplasmic inclusions, and it is suggested that the cytoskeleton participates in the evolution of the cytoplasmic inclusions.
    Materialart: Digitale Medien
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  • 25
    ISSN: 1432-0878
    Schlagwort(e): Key words Chondrocyte ; Synoviocyte ; Co-culture ; Proliferation ; Lipid peroxidation ; Cytotoxicity ; Ultrastructure ; Rat (Wistar)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract  Objective: A new co-culture system of rat articular chondrocytes and synoviocytes (HIG-82; cell line) was incubated with phorbol myristate acetate (PMA), H2O2 or a combination of Fe2+ and ascorbic acid to simulate inflammation-like radical attacks in articular joints. Methods: Chondrocytes were characterized by immunocytochemistry against collagen type II, transmission electron (TEM) and light microscopy. Lipid peroxidation was investigated by measuring thiobarbituric-acid-reactive material in the supernatants, cytotoxicity by determining release of lactate dehydrogenase and proliferation by measuring [3H]thymidine incorporation, culture protein and DNA. Results: PMA or Fe2+ and ascorbic acid induced lipid peroxidation in chondrocytes and synoviocytes that was decreased significantly in co-cultures. PMA and H2O2 dose dependently induced release of lactate dehydrogenase in chondrocytes, which was lowered in co-cultures or in previously co-cultured chondrocytes to a nearly basal level. In contrast, conditioned media of synoviocyte cultures showed no lowering effect on the radical-induced toxicity. Protection against H2O2-induced damage of cellular membranes by co-culturing was also shown by TEM. Synoviocytes released chondrocyte-stimulating growth factors spontaneously without previous interaction. Conclusion: Chondrocytes establish protective mechanisms against reactive oxygen species via an interaction with synoviocytes. Our co-culture model presents a possible way to study mechanisms of inflammation in articular joints under defined conditions.
    Materialart: Digitale Medien
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  • 26
    ISSN: 1437-773X
    Schlagwort(e): Key words KSHV ; HHV-8 ; TPA ; Ultrastructure ; Primary effusion lymphoma
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract The ultrastructure of Kaposi's sarcoma-associated herpesvirus (KSHV)/human herpesvirus-8 (HHV-8) has not yet been fully elucidated, although some findings have been reported using primary effusion lymphoma (PEL) cell lines, KS-1, harboring no Epstein–Barr virus (EBV) coinfection. In the present study, detailed fine structural examination of KSHV/HHV-8 was performed after stimulation of the PEL-derived cell line KS-1 with 12-O-tetradecanoyl-phorbol-13-acetate (TPA) in vitro. While unstimulated KS-1 cells contained a small number of intranuclear virus particles associated with no extracellular mature particles, KS-1 cells stimulated with TPA produced many extracellular mature particles as well as intranuclear particles, in addition to interesting tubulo-reticular structures and aggregated tubular structures in vesicles. The induced intranuclear particles were empty, doughnut shaped, and dense cored, with outer and inner diameters of 100–110 nm and 60–70 nm, respectively. Dense-cored extracellular mature particles were 150–160 nm in diameter, and some contained doughnut-shaped cores, together with a few megaloviruses, 260 nm in outer diameter. These findings indicate that KS-1 cells treated with TPA can produce extracellular mature particles as well as intranuclear particles, which were proven to be KSHV/HHV-8.
    Materialart: Digitale Medien
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  • 27
    ISSN: 1437-773X
    Schlagwort(e): Key words pHGF ; HGF ; Acute liver injury ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract The protective effect of hepatocyte growth-promoting factor (pHGF) against CCl4-induced acute hepatitis in rats was examined by light and electron microscopy. Hepatocyte growth-promoting factor, purified from infant pig liver in an active form, has been used clinically in patients with hepatitis in China. Four hours after administration of CCl4, a single dose of pHGF was administered intraperitoneally. Six hours after administration of CCl4, inhibition of CCl4-induced hepatic necrosis and hepatocytes with severely dilated endoplasmic reticula were evident in rats treated with pHGF. At 48 h post administration, most hepatocytes had recovered, and not only mitotic hepatocytes (10–13 mitotic cells/100) but also mitotic Kupffer cells were observed. At 72 h, it was evident that the differentiation of hepatic stellate cells (Ito cell) into myofibroblast-like cells and the development of fibrosis around the central veins was prevented by pHGF. These results suggested that (1) pHGF may stabilize cell membranes, (2) pHGF acts as a mitogen not only for hepatocytes but also for Kupffer cells, and (3) pHGF prevents fibrogenesis in the case of CCl4-induced liver injury by preventing the differentiation of hepatic stellate cells.
    Materialart: Digitale Medien
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  • 28
    ISSN: 1437-773X
    Schlagwort(e): Key words Heart ; Ultrastructure ; Capillaries ; Endothelium ; Stereology ; Cardioplegic solutions
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract In open heart surgery and transplantation, sufficient structural preservation of the myocardium immediately following cardioplegic arrest is a precondition for overcoming ischemia and for resumption of postischemic function. Therefore, we compared the protective effect of three clinically applied cardioplegic solutions with fibrillating and beating hearts using structural criteria. Left ventricular samples were taken from (1) beating, or (2) fibrillating or arrested hearts following coronary perfu-sion with (3) St. Thomas' Hospital solution, (4) histidine tryptophane ketoglutalate (HTK) (Custodiol), or (5) University of Wisconsin (UW) solution and fixed by immersion. Ultrastructural differences in the swelling of capillary endothelial cells and myocytes were quantitatively evaluated using stereological methods. Endothelial cells were somewhat more swollen after St. Thomas perfusion than those in beating and fibrillating hearts. HTK-arrested hearts showed significantly lower values for cellular edema than beating hearts. UW perfusion resulted in the (significantly) lowest degree of endothelial cell edema. Edematous changes in myocytes were significantly greater in St. Thomas-arrested hearts than in UW- or HTK-arrested hearts. Cardiomyocyte edema in beating and fibrillating hearts was comparable to that in St. Thomas-perfused hearts. Thus, the stereol-ogical analysis revealed significant differences between cardioplegic solutions in structural preservation of myocardial ultrastructure.
    Materialart: Digitale Medien
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  • 29
    Digitale Medien
    Digitale Medien
    Springer
    Medical electron microscopy 32 (1999), S. 175-183 
    ISSN: 1437-773X
    Schlagwort(e): Key words Cerebral blood flow ; Blood–brain barrier ; Repeated brief cerebral ischemia ; Hippocampal CA1 ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Neuronal damage and changes in cerebral blood flow (CBF) and the permeability of the blood–brain barrier (BBB) following repeated brief periods of ischemia were studied in Mongolian gerbils. The cerebral ischemia was produced by three repeated occlusions of bilateral common carotid arteries for 3 min at 1-h intervals. CBF and permeability of the BBB were examined with tracers (China ink and silver nitrate) at 1, 3, and 7 days post ischemia using light and electron microscopy. Three days after the reperfusion, significant extravasation of tracers, consequential reduction of CBF, extensive neuronal destruction, and intravascular platelet aggregation were observed. Such vascular changes in the CA1 region were more severe than those in the frontal cortex. These findings strongly support the view that microcirculatory disturbance may be a mechanism responsible for delayed neuronal death in the CA1 region of the hippocampus.
    Materialart: Digitale Medien
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  • 30
    ISSN: 1437-773X
    Schlagwort(e): Key words: Secretory carcinoma ; Breast ; Intracytoplasmic lumina ; Immnohistochemistry ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract We report a rare case of secretory carcinoma of the breast in a 50-year-old Japanese woman. The patient had been aware of a right breast tumor for 8 years, but had left it untreated. The tumor enlarged in size and became painful, and she visited our hospital. Breast carcinoma was diagnosed, and mastectomy was performed. Histopathological examination revealed features of a secretory carcinoma characterized by prominent secretory activity in the glandular and microcystic spaces, with some areas showing a follicular pattern resembling the thyroid gland. The secretory material was PAS-positive and immunohistochemically α-lactalbumin-positive. Ultrastructurally, the tumor cell contained many secretory vacuoles in the cytoplasm. In addition, extracellular and intracytoplasmic lumina were conspicuous; these were lined by microvilli projection and contained secretory material. By flow cytometric analysis, the DNA index was 1.14, which was diploid, showing relatively low proliferative activity.
    Materialart: Digitale Medien
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  • 31
    ISSN: 1432-0878
    Schlagwort(e): Key words Melanin-concentrating hormone neurons ; Lateral hypothalamic slice culture ; Immunocytochemistry ; Ultrastructure ; In situ hybridization ; Competitive RT-PCR ; Leptin assay ; Rat (Sprague Dawley)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract  Hypothalamic slices containing the lateral hypothalamic area (LHA) were prepared from 6- to 8-day-old rats and maintained in stationary culture for up to 35 days in order to analyse how well the melanin-concentrating hormone (MCH) neurons survived. As previously reported for other brain areas, this method yielded a long-term well-preserved organotypic organization. Light- and electron-microscopic investigations showed that differentiation continued and that synaptic contacts developed in vitro. After a period of elimination of damaged cells and fibres, most of the remaining neurons and glial cells retained a normal morphology throughout the culture period. MCH neurons, in particular, survived well as attested by the strong immunocytochemical and in situ hybridization signals still observed after several weeks. In a comparison with the day of explantation, competitive reverse transcription/polymerase chain reaction demonstrated the remarkable stability of the level of MCH mRNA at least until the 20th day in culture; after 30 days, the clear decrease in this level seemed to be correlated with a loss of MCH neurons, rather than with a decrease in MCH expression. After 10 days of culture, the incubation of slices in the presence of the hormone leptin (50 ng/ml) resulted in a strong decrease of MCH gene expression, suggesting that MCH neurons retained their physiological properties. Thus, the LHA slice stationary culture, especially between one and three weeks (i.e. after tissue stabilization and before extensive cell loss), appears to be a suitable method for physiological and pharmacological studies of these neurons.
    Materialart: Digitale Medien
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  • 32
    ISSN: 1432-0878
    Schlagwort(e): Key words Mechanoreceptors ; Synaptic proteins ; Histochemistry ; Ultrastructure ; Slit sensilla ; Hair sensilla ; Cupiennius salei (Chelicerata)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract Indirect immunocytochemical tests were used at the light- and electron-microscopic levels to investigate peripheral chemical synapses in identified sensory neurons of two types of cuticular mechanosensors in the spider Cupiennius salei Keys.: (1) in the lyriform slit-sense organ VS-3 (comprising 7–8 cuticular slits, each innervated by 2 bipolar sensory neurons) and (2) in tactile hair sensilla (each supplied with 3 bipolar sensory cells). All these neurons are mechanosensitive. Application of a monoclonal antibody against Drosophila synapsin revealed clear punctate immunofluorescence in whole-mount preparations of both mechanoreceptor types. The size and overall distribution of immunoreactive puncta suggested that these were labeled presynaptic sites. Immunofluorescent puncta were 0.5–6.8 μm long and located 0.5–6.6 μm apart from each other. They were concentrated at the initial axon segments of the sensory neurons, while the somata and the dendritic regions showed fewer puncta. Western blot analysis with the same synapsin antibody against samples of spider sensory hypodermis and against samples from the central nervous system revealed a characteristic doublet band at 72 kDa and 75 kDa, corresponding to the apparent molecular mass of synapsin in Drosophila and in mammals. Conventional transmissionelectron-microscopic staining demonstrated that numerous chemical synapses (with at least 2 vesicle types) were present at these mechanosensory neurons and their surrounding glial sheath. The distribution of these synapses corresponded to our immunofluorescence results.Ultrastructural examination of anti-synapsin-stained neurons confirmed that reaction product was associated with synaptic vesicles. We assume that the peripheral synaptic contacts originate from efferents that could exert a complex modulatory influence on mechanosensory activity.
    Materialart: Digitale Medien
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  • 33
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 11-16 
    ISSN: 0935-6304
    Schlagwort(e): Pyrolysis gas chromatography ; microstructure determination ; syndiotactic copolymers ; styrenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The composition and microstructure of syndiotactic para-methylstyrene/styrene copolymer was determined by a pyrolysis gas chromatography (Py-GC) method. This method uses the styrene and para-methylstyrene monomer peak intensities to determine the styrene and para-methylstyrene composition in the copolymer. The number average sequence length of styrene was calculated by using the triad peak intensities. Because of the low concentration of para-methylstyrene in the copolymer, the number average sequence length of para-methylstyrene was determined with formulas that incorporate the copolymer composition and the number average sequence length of styrene. The distribution of para-methylstyrene defined by the terms “percent of single units” and “percent of desired distribution” was calculated by the number average sequence of para-methylstyrene. This method has been tested with copolymers containing up to 24 mole% of para-methylstyrene. The composition results from Py-GC of para-methylstyrene and styrene copolymers used in this study were in excellent agreement with 1H-NMR results.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 34
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 24-28 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; ECD ; Micro-ECD ; GC detector ; organochlorine pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A new ECD, the HP 6890 Series Micro-ECD, was designed to address inherent deficiencies in classical electron capture detectors (ECD), especially with respect to sensitivity, linearity, dynamic range, and ruggedness. Several novel technologies were incorporated in the totally new design and were refined through practical testing and user feedback. Validation of the micro-ECD performance was accomplished through side-by-side testing of the Micro-ECD with previous ECDs following US EPA Contract Laboratory Program methods for pesticides and PCBs. In addition, extensive interviews were conducted with early users of the Micro-ECD who also had experience with other designs running a variety of ECD methods. The design and resulting performance improvements are described.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 35
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 33-38 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrophoresis ; chiral separation ; negatively charged chiral selectors ; capillary filling methods ; dual systems ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Data on the use of two chiral selectors, namely 18-crown-6 tetracarboxylic acid and a negatively charged cyclodextrin derivative (sulfated-β-cyclodextrin or carboxymethyl-β-cyclodextrin), in the same background electrolyte are presented. The use of such dual systems has a considerable influence on the resolution, as illustrated for the separation of tryptophan derivatives. Reduction of the consumption of chiral selector without significant loss in resolution was obtained by only partly filling the capillary and applying a run buffer without selector. This is illustrated for the chiral separation of tryptophan hydroxamate and the diastereomeric and enantiomeric separation of the dipeptide α/b-AspPhe-OMe.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 36
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 43-46 
    ISSN: 0935-6304
    Schlagwort(e): Green and roasted coffee ; diterpenes ; cafestol ; kahweol ; 16-O-methylcafestol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The three coffee diterpenes cafestol, kahweol, and 16-O-methylcafestol are mostly esterified with fatty acids. Little has been published about the diterpenes occurring in the free form. By means of gel permeation chromatography on Bio Beads S-X3, it is now possible to simultaneously analyze and quantify the small amounts of these compounds by RP-HPLC. In this way, free kahweol was first proved to be an ingredient of Robusta coffee. Various Arabica and Robusta coffees - both green and roasted - were investigated. Free diterpenes were found in green coffees in amounts below 200 mg/kg dry matter. In comparison to the respective total diterpene content determined by the same HPLC method after saponification of the coffee oil, the proportion of free diterpenes ranged from 0.7 to 3.5 %. During the roasting process, the three uncombined diterpenes behaved similarly: free 16-O-methylcafestol, cafestol as well as kahweol were degraded with increasing roasting temperature.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 37
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 52-54 
    ISSN: 0935-6304
    Schlagwort(e): Ethanol ; mobile phase ; factorial planning ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 38
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 63-66 
    ISSN: 0935-6304
    Schlagwort(e): Divinylbenzene copolymers ; exclusion limit ; size exclusion chromatography ; surface area ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 39
    ISSN: 0935-6304
    Schlagwort(e): RP-HPLC ; GC-MS ; trioxanes ; thermolysis products ; quantitative analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 40
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 131-132 
    ISSN: 0935-6304
    Schlagwort(e): RP-HPLC ; theophylline ; asthma ; apnea ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 41
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 153-158 
    ISSN: 0935-6304
    Schlagwort(e): Vapor analysis ; nerve agents ; sulfur mustard ; data acquisition ; automation ; valve injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A method is presented for the continuous analysis of generated vapors of the nerve agents soman and sarin and the blistering agent sulfur mustard. By using a gas sampling valve and a very short (15 cm) column connected to an on-column injector with a “standard length” column, the system can either be calibrated or used for performing high speed gas analyses. When using a flame ionization detector, the detection limit was ca. 100 ppb (ca. 0.5-1.0 mg/m3). This technique is applied in inhalation toxicokinetic studies of nerve agents and mustard gas in the guinea pig.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 42
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 149-152 
    ISSN: 0935-6304
    Schlagwort(e): Large volume on-column injection ; flooded zone ; capacity of 0.53 mm i. d. precolumns ; solvent trapping ; solvent vapor exit ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---0.53 mm i. d. uncoated precolumns of about 10 m in length followed by a solvent vapor exit have become a standard set-up for large volume on-column injection. It went unnoticed, however, that the introduction of a vapor exit requires two modification of previous working guidelines. First, the capacity of the precolumn to retain sample liquid is increased by a factor of 2.3-3 as a result of the around 100 times higher carrier gas flow rate. Secondly, it must be considered that this gain in retention of liquid is lost again upon closure of the exit: as the gas flow rate is reduced to a few mL/min, the layer of the residual sample liquid expands about 2.3-3 times. Hence, closure should occur late, and a section of the precolumn must be assigned for this secondary spreading.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 43
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 177-180 
    ISSN: 0935-6304
    Schlagwort(e): Fresh water systems ; burbot ; organotin compounds ; speciation analysis ; GC-AED ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 44
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 93-96 
    ISSN: 0935-6304
    Schlagwort(e): Capillary GC ; PTV and on-column injectors ; milk fat triglycerides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The PTV (Programmable Temperature Vaporizer) is a split/splitless injector which allows the sample to be introduced at a relatively low temperature, thus affording accurate and reproducible sampling. After injection the PTV is rapidly heated to transfer the vaporized components into the capillary column. This type of injector has proved to be an efficient tool for the evaluation of fatty acids, essential oils, and pesticides in food analysis. In this work the suitability of PTV for the analysis of milk fat purity by the Official EU method was evaluated. This method is based on the gas chromatographic determination of triglycerides only according to their total number of carbon atoms followed by the application of formulae deriving from multiple linear regressions. The analysis is currently carried out with a packed column or a short capillary column and an on-column injection system. Several samples of pure milk fat and mixtures of milk fat with foreign fat were analyzed with the same capillary column and by using both PTV and on-column injection systems. The results show that the gas chromatographic profile obtained by PTV is comparable with that obtained by the on-column injector, while repeatability and reproducibility data meet the requirements indicated in the Official Method. Therefore, this study demonstrates that it is possible to use the PTV instead of the on-column injector to determine the purity of milk fat with this method.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 45
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 188-190 
    ISSN: 0935-6304
    Schlagwort(e): LC stationary phases ; porous graphitic carbon ; surfactant ; alkyl glycosides ; glycosides ; evaporative light scattering detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 46
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 195-200 
    ISSN: 0935-6304
    Schlagwort(e): Multi-dimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; GC×GC ; BTEX ; aromatics ; reformulated gasoline ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Comprehensive two-dimensional gas chromatography (GC×GC) has been applied to the quantitative analysis of benzene, toluene, ethylbenzene, xylenes (BTEX), and all heavier aromatic compounds in gasoline. The two-dimensional chromatographic separation used volatility selection on the first-dimension column and polarity selection on the second-dimension column. In the resulting GC×GC chromatogram, aromatic species were resolved from other compound classes. Moreover, structurally related aromatics were grouped in a manner that facilitated identification and integration. The response of a flame ionization detector to each major aromatic group in gasoline was calibrated using internal standards. Quantitation produced results directly comparable with ASTM standard methods. The present GC×GC method can be expanded to analyze other gasoline components.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 47
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 205-212 
    ISSN: 0935-6304
    Schlagwort(e): Membrane extraction ; hollow fiber membrane ; thermodesorption ; GC-MS ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The range of application of a commercial thermodesorption-cryofocussing unit connected to a gas chromatograph/mass selective detector was extended to water analysis by using it in conjunction with membrane extraction. A flow of nitrogen passes through a silicone hollow fiber immersed in the water sample and extracted volatile organic compounds are enriched in a sorption tube mounted on top of the extraction cell. The sorption tube is then placed in the thermodesorption unit and analyzed by GC/MS. The optimal extraction parameters of this combined method were found to be 30 min extraction at 20°C with a stirring speed of 1,250 rpm and a flow rate of 100 mL/min nitrogen using a silicone hollow fiber of 0.3 m length. Under these conditions the reproducibility of the method was 5.2-10.5% RSD. The linear dynamic range of the optimized method spans three orders of magnitude and detection limits were found to be 0.02-0.1 μg/L for cis/trans-1,2-dichloroethene, benzene, trichloroethene, chlorobenzene, bromobenzene, ethylbenzene, 1,1,2,2-tetrachloroethane, and 1,2/1,4-dichlorobenzene. The method was found to be suitable for compounds with boiling points up to 220°C as memory effects increased considerably from dichloro- to hexachlorobenzene. Highly contaminated groundwater samples were analyzed. Quantitative results corresponded well with those achieved with conventional headspace-GC/FID.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
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  • 48
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 222-224 
    ISSN: 0935-6304
    Schlagwort(e): High-performance liquid chromatography ; Artemisia capillaris ; phenolic compounds separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 49
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 217-221 
    ISSN: 0935-6304
    Schlagwort(e): HPLC ; UV detection ; linear range ; method validation ; Beer-Lambert law ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Determination of the linear range is one of the main concerns in validation of an HPLC analysis method. It is particularly important since single point calibration will be then used routinely. We proposed an iterative methodology to handle this problem. The idea was, at each step, to test statistically whether the following point belonged to the same regression line. The methodology was then used to evaluate quantitatively the effect on linear range of a shift in detection wavelength or of the detector bandwidth. Although experimental results were globally in accordance with spectroscopic theory, magnitudes observed were rather large. So the linear range could vary by a factor of over 2 with changes in conditions that remained within the range of current practical values. Changes in detection wavelength were limited to about fifteen nm around λmax and the detector used was considered to be representative of modern high-performance UV detectors. The question of how to take consequences in method validation into account was raised. The solution proposed recommended that the validation was undertaken in conditions as close as possible to those where the method would be conducted routinely. This means with the same instrumentation and on the product of interest for analyses.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 50
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 231-234 
    ISSN: 0935-6304
    Schlagwort(e): Trace analysis ; air samples ; BTX ; equilibrium-sorptive enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 51
    ISSN: 0935-6304
    Schlagwort(e): Tebuthiuron ; GC-MS ; HPLC ; drinking water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 52
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 245-246 
    ISSN: 0935-6304
    Schlagwort(e): Chloride ; suppressed ion chromatography ; concrete ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 53
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 251-255 
    ISSN: 0935-6304
    Schlagwort(e): Multi-dimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; GC × GC ; mass spectrometry ; petroleum ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Comprehensive two-dimensional gas chromatography coupled with mass spectrometric detection (GC × GC/MS) is a three-dimensional analytical method. In its application to petroleum analysis, the high peak capacity of GC × GC produced chromatographic resolution of over 750 peaks from a marine diesel fuel. The MS detector provided a full-scan mass spectrum for each resolved peak. The integration of an MS detector with GC × GC provides increased capability to identify minor components, determine members of homologous series, and characterize ordered peak patterns of related components that are visible in the GC × GC chromatogram.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 54
    ISSN: 0935-6304
    Schlagwort(e): Molecular imprinting ; PAH ; molecular recognition ; selectivity ; redox polymerization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A non-covalent type of molecular imprinting effect toward a polyaromatic hydrocarbon (PAH), viz. anthracene, was studied utilizing uniformly sized ethylene dimethacrylate (EDMA) polymer particles without functional host monomers. Although polymerization at 0°C initiated by a redox initiation system was expected to afford larger molecular imprinting effect due to stronger and more effective intermolecular interaction between the template and surface functional groups of the polymer, almost no imprinting effect was observed, while a much higher polymerization temperature of 70°C unexpectedly afforded a larger molecular imprinting effect for the template anthracene. In order to determine the unexpected imprinting effects observed, uniformly sized, macroporous un-imprinting EDMA polymer particles (base particles) were prepared by various polymerization techniques at different polymerization temperature as well as with different initiation systems. The careful studies proved that each kind of base polymer particle showed different molecular recognition ability, especially toward anthracene, which is depends upon the physical properties of each kind of base polymer particle. On the basis of these facts, we would propose that the potential molecular recognition ability of the un-imprinted base polymer particles is another important factor for realization of effective molecular imprinting alongside the factors reported previously.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 55
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 276-278 
    ISSN: 0935-6304
    Schlagwort(e): Cyclic carbonates ; thermal stability ; chemical stability ; gas phase chromatography ; liquid phase chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 56
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 283-286 
    ISSN: 0935-6304
    Schlagwort(e): Evaporative light scattering detection ; capillary nebulizer ; packed capillary ; columns ; high temperature liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 57
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 303-304 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; food analysis ; pesticide residues ; thiabendazole ; imazalil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 58
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 305-307 
    ISSN: 0935-6304
    Schlagwort(e): High temperature gas chromatography ; chocolate analysis ; triacylglycerols determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 59
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 309-314 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; isomers ; pneumocandins ; separation ; transition metal ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The novel separation of a 3-hydroxyproline containing a semi-synthetic macrocyclic antifungal agent from its structurally related 4-hydroxyproline isomer using capillary electrochromatography (CEC) is described. The molecular weight of the two compounds is 1093 Daltons and they differ only in the placement of a proline -OH group. The separation is achieved using capillaries packed or coated with ODS particles (C18) or with glycerol bound to silica through a carbon chain linker. The presence of a transition metal (Ni(II), Ag(I), Zn(II), or Cu(II)) as buffer additive in the phosphate buffer (pH=2.5):CH3CN (75:25, v/v) is essential to achieve a baseline separation. HPLC columns packed with similar ODS particles showed no selectivity. Capillaries packed or coated with C18 material under similar conditions showed partial selectivity compared to the glycerol capillaries. Some fundamental aspects of CEC, such as capillary temperature, applied voltage, and buffer composition were varied in order to study the mechanism of the separation. This mechanistic study included the testing of first and second row transition metal ions (individually or in combination), the use of organic solvents, the use of an ion pair reagent, and the use of β- and γ-cyclodextrin to assess the impact on the separation. The resolution was dependent on the metal ion concentration and is consistent with a mechanism of metal-oxygen complexation through the hydroxyl groups of the two isomers and glycerol.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 60
    ISSN: 0935-6304
    Schlagwort(e): Solid phase microextraction (SPME) ; capillary gas chromatography ; detection limits ; wine aroma compounds ; classification of wines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Headspace-SPME followed by capillary gas chromatography/mass spectrometry was used to investigate 90 German wines originating from different grape varieties, vintages, and growing areas. Aromagrams obtained in single ion monitoring (SIM) and in the full scan detection mode (SCAN) of quadrupole mass spectrometer were compared. Detection limits, reproducibility, and linearity for some aroma relevant substances were estimated over a wide concentration range. The advantages of SIM data set (lower detection limit, better reproducibility and linearity in the smaller concentration ranges) should be reflected in more reliable results in classification of wines. To verify these expectation, classification of variety by discriminant analysis was performed with cross validation using both SIM and SCAN data sets including 19 aroma compounds, respectively.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 61
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 335-338 
    ISSN: 0935-6304
    Schlagwort(e): Capillary GC trace analysis of C2-C4 hydrocarbons ; signal-to-noise ratio, improvement ; post column cryogenic trapping ; thermal remobilization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A method for the improvement of signal-to-noise ratios and hence detection limits in capillary gas chromatographic trace analysis of C2-C4 hydrocarbons was developed. It is based on the post column cryogenic trapping of the separated hydrocarbons using liquid nitrogen as coolant and its fast reinjection into the detector by rapid heating of the capillary tubing used for trapping. The improved signal-to-noise ratios were applied to decrease the sample volume and/or to lower the detection limit 10 to 27 times. The concentrations of these hydrocarbons in an urban air sample determined without and with post column cryogenic trapping were in good agreement but the precision was better when applying the cryogenic trapping mode.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 62
    ISSN: 0935-6304
    Schlagwort(e): Multidimensional GC ; enantioselective gas chromatography ; lemon oil ; monoterpene hydrocarbons ; monoterpene alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This paper describes a fully automated, multidimensional, double-oven GC-GC system, developed in our laboratory. The system is based on the use of mechanical valves which allow the multitransfer of different fractions during the same GC analysis and the use of the two GC independently when the multitransfer options is not used. Pneumatic and electronic circuits permit maintenance of constant retention times in the pre-column, even for the components eluted after numerous transfers. The system has been used for the determination of the enantiomeric distribution of β-pinene, sabinene, limonene, linalol, terpinen-4-ol, and α-terpineol in lemon oils. The results obtained allowed the characterization of cold-pressed lemon oils.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 63
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 362-366 
    ISSN: 0935-6304
    Schlagwort(e): Pentafluorophenyldimethylsilyl (flophemesyl) chloride ; split and splitless injection ; derivatised sterol analysis ; synthetic pyrethroids ; injector liner activity ; gas chromatographic electron capture detection ; multidimensional gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 64
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 367-372 
    ISSN: 0935-6304
    Schlagwort(e): Sweeping ; sample stacking ; micellar electrokinetic chromatography (MEKC) ; retention factor (k) ; sample matrix ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The concept of sweeping has been used in electrokinetic chromatography to explain the concentrating mechanism in micellar electrokinetic chromatography when the sample matrix is a high resistivity non-micellar aqueous solution. Theoretical and experimental studies were undertaken. It was found that the total focusing effect is brought about by the cumulative effect of sweeping and sample stacking. For better analytical results, compounds showing low to moderate retention factors (k) and compounds showing high values of k must be dissolved in low and high conductivity matrices, respectively.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 65
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 379-385 
    ISSN: 0935-6304
    Schlagwort(e): CZE ; indirect UV detection ; anions and organic acids ; environmental samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Capillary zone electrophoresis (CZE) with indirect UV detection was developed for the simultaneous determination of inorganic anions and organic acids in environmental samples. Various aromatic acids (benzoic, phthalic, trimellitic, and pyromellitic acids) were evaluated as background electrolytes (BGEs) to give high resolution and detection sensitivity. Co-electroosmotic conditions such as the concentration of BGE, electrolyte pH, and EOF modifier were systematically investigated. Three inorganic anions and ten organic acids were determined simultaneously in 10 min using an electrolyte containing 10 mM phthalic acid, 0.5 mM myristyltrimethylammonium bromide (MTAB), and 5% methanol (MeOH) (v/v) at pH 5.60. Linear plots for the test solutes were obtained in the concentration range 0.01-1.0 mM with detection limits in the range 5-30 μM. The proposed method was successfully demonstrated for the determination of inorganic anions and organic acids in natural water, soil, and plant extracts after direct sample injection.
    Zusätzliches Material: 7 Ill.
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  • 66
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 395-402 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; pulsed splitless injection ; pesticide residues ; matrix effects ; retention gap ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The applicability of pulsed splitless injection to the gas chromatographic analysis of pesticide residues in fruit and vegetables has been evaluated. 22 pesticides belonging to different chemical classes, including those known to be liable to matrix induced response enhancement, were selected for the study. The parameters of pressure pulse have been tested for optimum performance of injection. Application of the pressure pulse was found to decrease matrix effects during analyses of real samples. Further decline of matrix effects was obtained using higher sample injection volumes. The installation of a deactivated retention gap was necessary to obtain good peak shapes with injection volumes exceeding 1 μL of sample. Up to 4 μL was then injected without peak distortion and consequent loss of resolution. Using 4 μL pulsed splitless injection, matrix effects were almost completely eliminated even at very low concentration levels of analytes. The highest matrix effects observed for tested compounds at the lowest concentration level tested were in the range of 110-122%.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 67
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 403-413 
    ISSN: 0935-6304
    Schlagwort(e): Constant length optimization ; constant efficiency optimization ; efficiency-optimized flow rate ; fast GC ; film inefficiency factor ; high pressure drop ; speed-optimized flow rate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: At the high pressure drop required for the fast analysis of complex mixtures, the equations for the column plate height, H, and plate duration, Q, as functions of the carrier gas velocity, u, differ substantially from the equations for the same quantities expressed via the carrier gas flow rate, F. While u as an independent pneumatic variable is more convenient for the theoretical studies, F is a more convenient as a control parameter in practical applications. Equations for H vs. u and for Q vs. u from Parts 1 and 2 are transformed here into expressions for H vs. F and Q vs. F. An efficiency-optimized flow rate (EOF) and a speed-optimized flow rate (SOF) are found. Expressions for these two quantities are considerably simpler than their velocity-based counterparts. In particular, SOF does not depend on column length, film thickness, and pressure drop.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 68
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 417-420 
    ISSN: 0935-6304
    Schlagwort(e): Sample preparation ; nitrophenols ; PCP ; 2,4-D ; liquid chromatography ; supported-liquid-membrane extraction ; environmental monitoring ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 69
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 427-428 
    ISSN: 0935-6304
    Schlagwort(e): p-Chlorophenol ; urine ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 70
    ISSN: 0935-6304
    Schlagwort(e): Mycotoxin ; T2 ; solid phase microextraction ; GC/FID ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 71
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 339-342 
    ISSN: 0935-6304
    Schlagwort(e): Chlorophyll ; SFC ; supercritical fluid chromatography ; vegetables ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Complex mixtures of chlorophyll degradation products may arise during processing and storage of vegetable oil and green plant materials like broccoli and spinach. Determination of these compounds is important in the area of food chemistry. Therefore a method using packed column supercritical fluid chromatography (SFC) has been developed. The method comprises chromatography using a simple gradient of methanol in carbon dioxide at constant column back pressure of 30 MPa and a column temperature of 40°C. Effects of pressure and mobile phase composition showed the importance of applying a modifier gradient for optimal separation of the chlorophyll products. The method permits separation of 15 chlorophyll derivatives including chlorophyll a and b, pheophytins, and pyropheophytins on a C18 column in about 20 minutes. Identifications of the individual peaks were based on reference compounds, the retention order of the compounds, and their absorption spectra.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 72
    ISSN: 0935-6304
    Schlagwort(e): Capillary gas chromatography ; gas chromatography-mass spectrometry ; essential oil analysis ; Lepechinia schiedeana ; antioxidant activity ; lipid peroxidation ; Ledol; Ledol HMQC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Steam distillation (SD), simultaneous distillation-solvent extraction (SDE), microwave-assisted solvent extraction (MWE), and supercritical (CO2) extraction (SFE) were used to isolate secondary metabolites from Lepechinia schiedeana. The various extracts were analyzed by capillary gas-chromatography, on poly (dimethylsiloxane) (DB-1) and poly(ethyleneglycol) (INNOWAX), 60 m columns, using FID or MSD (EI, 70 eV). Kováts indexes, mass spectra, or standard compounds were employed for compound identification. 43, 61, 67, and 79 compounds at concentrations above 0.01% were detected in the SD, SDE, MWE, and SFE extracts, respectively. Ledol, C15H26O, was the major constituent (20.04-36.87%) in all extracts. Oxygenated sesquiterpenes (24.36-43.14%), C10H16, monoterpenes (27.70-39.87%), and C15H24, sesquiterpenes (10.04-22.22%) were the main groups of compounds present in SD, SDE, MWE, and SFE extracts. Heavy hydrocarbons (Cn 〉 15), diterpenoids, and phytosterols were found only in MWE and SFE extracts. The antioxidant activity of Lepechinia schiedeana was measured by the HRGC quantification of the volatile carbonyl compounds, final products of lipoxidation, released in a model lipid system (sunflower oil) by the effect of the Fenton reagent. The concentration of volatile carbonyl compounds decreased by 65% when lipid oxidation was induced in the presence of macerated Lepechinia plant. The protection of polyunsaturated acids in sunflower oil was also studied by measuring their concentrations after heating of the oil (180°C, 2 h) with and without macerated Lepechinia plant.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 73
    ISSN: 0935-6304
    Schlagwort(e): Silver ion HPLC ; long chain polyunsaturated fatty acid ; isopropanol ; separation of positional isomers ; degree of unsaturation ; normal phase retention effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A high resolution approach to silver ion HPLC was studied for the separation of positional isomers of triacylglycerols (TAGs) containing long chain polyunsaturated fatty acids (PUFA) such as eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and docosapentaenoic acid (DPA) in enzymatically synthesized structured TAGs. Isopropanol was used as a novel modifier in a hexane-acetonitrile based mobile phase for silver ion HPLC. Peak identification was based on HPLC-mass spectroscopy and selectivities of lipases. Positional isomers of TAGs containing one molecule of EPA, DHA, or DPA with saturated fatty acids (FAs) such as caprylic acid and palmitic acid were separated within 13 min using a gradient of hexane-isopropanol-acetonitrile as mobile phase. TAGs containing two or more EPA, DHA, or DPA were also separated from each other within 25 min, but their positional isomers were unresolved. The retention characteristics of the TAG were found to be related to the number of carbon atoms in the FAs present in addition to the number of double bonds and their isomeric configuration. One isomer with an unsaturated FA in the sn-2 position eluted faster than the other with the unsaturated FA in the sn-1 or 3 position. Species with longer chain FAs attached to TAGs with the same degree of unsaturation eluted faster than those that have shorter chain FAs. For example, docosapentaenoylhexadecanoyloctanoin (DPA/C16/C8) was eluted faster than dioctanoyldocosapentaenoin (DPA/C8/C8).
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 74
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 373-378 
    ISSN: 0935-6304
    Schlagwort(e): Electrophoresis ; electrophoretic mobilities ; CZE ; MEKC ; peptides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A computer model is presented for the prediction of the electrophoretic mobilities of peptides from physical constants derived from their amino acid sequences. The model assumes that the electrophoretic mobility can be represented by a product of four functions according to the relation:  lcomp= l(L)w(W)q(Q)c(CC), where L (a length parameter) is represented by the number of amino acid residues of the peptide, W (a width parameter) is represented by the average residue mass, Q = the charge of the peptide, and CC = the position of the center of charge relative to the center of mass. The model was used to calculate the electrophoretic mobilities of peptides in a 50 mM phosphate buffer at pH 2.5. Sixty-four test peptides ranging in size from 2 to 39 amino acid residues were used for this study. The calculated mobilities show excellent correlation with experimental measurements with a correlation coefficient greater than 0.98.
    Zusätzliches Material: 5 Tab.
    Materialart: Digitale Medien
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  • 75
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 386-390 
    ISSN: 0935-6304
    Schlagwort(e): Sulfur chemiluminescence detection ; sulfur simulated distillation ; boiling point distribution ; simultaneous FID/SCD analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A gas chromatographic system for the simultaneous acquisition of hydrocarbon and sulfur chromatograms was developed. Detection of sulfur compounds is achieved using a sulfur chemiluminescence detector (SCD) mounted in series with a flame ionization detector (FID). A constant fraction of the effluent of the FID is transferred to the SCD by means of a fixed restrictor. Unlike previous versions of this approach, the FID is not used to generate the chemiluminescent sulfur species. Rather, the FID is operated under optimum conditions for hydrocarbon analysis and a furnace is used to generate the chemiluminescent sulfur species. The system permits dual acquisition of the hydrocarbon and sulfur signals in a single analysis with a single column, since the detectors are operated in a serial fashion. The application of sulfur simulated distillation using this approach was examined, since this requires simultaneous universal and sulfur selective detection. Precision of absolute response of both the FID and SCD was typically less than 2% RSD for a standard reference material.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 76
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 391-394 
    ISSN: 0935-6304
    Schlagwort(e): REMPI-TOFMS ; laser mass spectrometry ; supersonic jet ; GC-MS ; interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The laser-based methods Laser Induced Fluorescence (LIF) and Resonance-Enhanced Multi-Photon Ionization (REMPI) can be used as highly selective detection modes for gas chromatography (GC). One major prerequisite for successful application of these detection methods is the availability of appropriate and reliable interfaces between the GC effluent and the molecular beam inlet. When a pulsed supersonic molecular beam (jet) source is used, the analyte molecules are efficiently cooled, allowing maximum selectivity of the laser spectroscopic detection methods. However, several technical problems have to be solved for practical realization of a GC-supersonic jet valve hyphenation. The pulsed jet interface should not interfere with the GC properties and the supersonic molecular beam properties. Further a good working cycle for the conversion from the continuously flowing GC current to the pulsed jet gas flow should be attained. This paper presents a novel setup of a GC-pulsed jet interface. The construction allows temporal and spatial compression of the analyte molecules in jet gas pulse and thus an increase of the detection sensitivity. Moreover, the GC effluent comes into contact only with glass surfaces and not with valve parts like plungers and seals. This reduces memory effects and sample decomposition. The valve setup is tested with a REMPI-TOFMS instrument.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 77
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 414-416 
    ISSN: 0935-6304
    Schlagwort(e): Selenium ; water ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A method for the selective determination of Se4+ and Se6+ using solid phase microextraction (SPME) and GC/MS analysis is presented. Se4+ is selectively derivatized by reaction with 4,5-dichloro-1,2-phenylenediamine to form the corresponding piazselenolo complex, extracted by the SPME fiber, and determined by GC/MS. The RSD at a 5 μg/L concentration was 9.88% and the theoretical detection limit 6 ng/L. The method was employed to test real matrices; tap and river water were analyzed before and after spiking giving a recovery rate of 102% in river water and 97% in tap water.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 78
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 421-423 
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective gas chromatography ; 2,3-di-O-methyl-6-O-tert-butyldimethylsilyl-β-cyclodextrin ; 2,3-di-O-acetyl-6-O-tert-butyldimethylsilyl-β-cyclodextrin ; γ-dithiolactones ; olfactometry ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 79
    ISSN: 0935-6304
    Schlagwort(e): HPLC ; nitrotyrosine ; nitrotocopherol ; analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---For three decades, high performance liquid chromatography has proven itself to be a powerful, flexible, and inexpensive tool for basic and clinical research. Recent advances in our understanding of disease have prompted a demand for more sensitive and selective methods of routine bioanalysis, particularly with respect to the determination of oxidative metabolites and biomarkers of oxidative stress. Multidimensional detectors utilizing coulometric arrays offer a solution to these research needs. The challenge to the bioanalyst is now to creatively apply HPLC-ECD technology to promising research and clinical enterprises.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 80
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 449-453 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrophoresis ; experimental design ; cyclodextrin ; chiral separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Orthogonal design and uniform design were used for the optimization of separation of enantiomers using 2,6-di-O-methyl-β-cyclodextrin (DM-β-CD) as a chiral selector by capillary zone electrophoresis. The concentration of DM-β-CD, buffer pH, running voltage, and capillary temperature were selected as variable parameters, their different effects on peak resolution were studied by the design methods. It was concluded that orthogonal design offers a rapid and efficient means for testing the importance of individual parameters and for determining the optimum operating conditions. However, for a large number of both factors and levels, uniform design is more efficient. The effect of addition of methanol and citric acid buffer on the separation of enantiomers was also examined.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 81
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 547-552 
    ISSN: 0935-6304
    Schlagwort(e): Water analysis ; polar pollutants ; solid-phase extraction ; chemically-modified polymeric resins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This study assesses how the physical characteristics of styrene-divinylbenzene (PS-DVB) resins affect the extent to which they are modified when they are functionalized, and how they affect recoveries in on-line solid-phase extraction (SPE) of some polar phenolic compounds, pesticides, and metabolites from water samples which were analyzed by liquid chromatography and UV detection. For this purpose, three commercial PS-DVB resins with different physical characteristics (Amberchrom GC-161m and two different PLRP-S resins) were chemically modified by placing a hydrophilic group, an o-carboxybenzoyl moiety, on their surface; although the physical characteristics are different, the extent of modification did not vary significantly. The results from the SPE process with each sorbent were related to their physical and chemical properties. The polymers with higher surface area provided better recoveries. Moreover, the recoveries for these analytes were better with the chemically-modified polymers due to the higher polarity of these sorbents. The best recovery values were with the sorbent obtained from the chemical modification of Amberchrom GC-161m, the commercial sorbent with higher surface area. For instance, in the analysis of 50 mL of a sample of 2 μg L-1, the recovery of phenol was 40% with Amberchrom GC-161m and 65% with the chemically-modified Amberchrom GC-161m.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 82
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 565-588 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Kovats retention index ; vapor pressure ; boiling point ; Wilson activity coefficient ; binary phase diagrams ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Non-ideal mixing in a dimethylsilicone stationary phase is modeled according to the Wilson activity coefficient. Pure liquid vapor pressures of alkylated compound series are calculated from capillary GLC retention with the functional group heat of solution in a polymer solvent. The new method uses the Kovats index, molar mass, and functional group to determine the bubble line of a compound. Boiling points at reduced and normal pressure are compared to literature values of 194 gasoline components. An unlike molecular pair interaction parameter is derived, using only bubble line data of the pure liquids. Binary phase diagrams are constructed and compared to vapor liquid equilibrium data.
    Zusätzliches Material: 22 Ill.
    Materialart: Digitale Medien
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  • 83
    ISSN: 0935-6304
    Schlagwort(e): Computer modeling of GC ; computer simulation of GC ; computer-assisted GC analysis ; GC multicolumn analysis ; heart cutting GC analysis ; computer-assisted column design ; computer-assisted selectivity tuning ; retention index mapping ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The analysis of four components in a mixture containing many possible interferents is simplified by heart-cutting serially connected columns containing stationary phases of widely different polarities. The design of the proper lengths of the two columns and timing the heart-cuts is accomplished with the aid of a computer simulation of the problem. The computer program calculates the proper lengths of column to produce the shortest analysis time and also outputs the predicted chromatograms from both columns. The chromatogram from the first column is used to construct the timing gates for the heart-cuts and the chromatogram from the second or analytical column is used to set integration gates for the selected compounds of interest.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 84
    ISSN: 0935-6304
    Schlagwort(e): Large volume injection ; packed capillary LC ; temperature programming ; retinyl esters ; vitamin A ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A non-aqueous isocratic reversed-phase packed capillary high performance liquid chromatography method for the determination of retinyl esters, utilizing temperature programming and on-column focusing large volume injection, has been developed. The stationary phase material was C30, and the mobile phase consisted of acetonitrile-dichloromethane (70 : 30, v/v). A three-step temperature program, starting at 10°C for 10 min, then 1°/min to 30°C, and finally 2.5°/min to 70°C, was found most appropriate. Compared to an isothermal separation at 25°C, this temperature program provided improved peak resolution, enhanced peak shapes of the last eluting compounds, and a reduction of the overall elution time. A mass limit of detection of 27 pg was found with respect to retinyl palmitate, using UV detection with an “U” shaped flow cell at 327 nm. This corresponds to a concentration limit of detection of 2.7 pg/μL, when utilizing an injection volume of 10 μL. The concentration of retinyl palmitate in arctic seal liver samples was estimated to be 62.6 μg/g liver.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 85
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 501-508 
    ISSN: 0935-6304
    Schlagwort(e): Fast GC ; film inefficiency factor ; high pressure drop ; thick film columns ; thin film columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The negative effect of the liquid stationary phase film thickness on the column efficiency is strongest for peaks with retention factors, k, in the vicinity of k = 0.3-0.4 and rapidly diminishes with the departure of k from that region. Additionally, at the high pressure drop required for fast analysis of complex mixtures, the negative effect of the same film thickness diminishes with the increase in column length, regardless of the k values. In practice, it is recommended to ignore the film thickness and optimize the columns as thin film ones regardless of their actual film thickness. Accounting for the film thickness results only in a modest improvement in the resolution for a few affected peaks - those with k = 0.3-0.4. However, this improvement comes at the cost of a substantial increase in analysis time, and should be used only as the action of the last resort.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 86
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 514-520 
    ISSN: 0935-6304
    Schlagwort(e): Solid-phase extraction ; high temperature - gas chromatography ; gas chromatography - mass spectrometry ; wax esters fennel seed oil ; caraway seed oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A rapid method for the isolation and quantitative determination of wax esters in vegetable oils was developed. For the first time wax esters in oils were separated from the triglyceride matrix by means of solid-phase extraction, which allows rapid sample preparation in parallel and therefore a high sample throughput. The thus obtained wax ester fractions of fennel and caraway seed oils were analyzed by high temperature gas chromatography. GC-MS analyses were carried out using electron impact ionization in order to characterize the wax ester fraction. With respect to the results of the GC-MS analyses different isomers of saturated wax esters with the same carbon number were observed. Additional monounsaturated wax esters with an unsaturated fatty acid moiety were identified.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 87
    ISSN: 0935-6304
    Schlagwort(e): Clusia criuva Cambess ; counter-current chromatography ; flavonoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The family Guttiferae belongs to the superorder Theiflorae, order Theales and according to Dahlgren's system of classification, it is equivalent to Hypericaceae (=Clusiaceae) [1]. This family consists of 49 genera encompassing over 1000 species of wide distribution in the tropics as shrubs and trees [2]. Plants of the genus Clusia have been used in folk medicine for the treatment of different kind of illness such as: febrifuge, anti rheumatic, purgative, for stomach problems and, in Brazil, they are very commonly used to heal wounds [3]. The key of any study of material from natural sources is the availability of suitable separation methods for the isolation of pure products [4-6]. Tentatives for separations using chomatography on solid support phases were not very efficients in the fractionation of Clusia criuva Cambess methanolic/ethyl acetate extracts. However, the use of counter-current chromatography, an all liquid technique, showed advantages in comparison with the more traditional liquid-solid separation methods and even with HPLC. In this sense it was possible to isolate flavonoid glycosides from ethyl acetate extract of Clusia criuva, in a very short operation time.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 88
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 541-546 
    ISSN: 0935-6304
    Schlagwort(e): Solvating gas chromatography ; gas chromatography ; fast separation ; pesticides ; herbicides ; aldehydes ; packed capillary columns ; polymer-encapsulated silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Rapid separations of selected environmentally important polar compounds using polymer-encapsulated silica stationary phases and a carbon dioxide mobile phase under solvating gas chromatography (SGC) conditions are reported. Ten underivatized short chain aldehydes and ten nitrogen-containing herbicides were separated within 1 min and 5 min, respectively, using a 30 cm×250 μm i. d. column packed with diol-bonded, polyethylenimine (PEI)-coated, and hexamethyldisilazane (HMDS)-end-capped silica particles (5 μm, 120 Å). Seven organophosphorus pesticides were resolved in less than 5 min using a 30 cm×250 μm i. d. column packed with polymethylhydrosiloxane-deactivated and SE-54 encapsulated silica particles. Separation numbers per unit time increased with pressure and temperature ramps. Both rapid pressure and temperature programming can be used to increase the speed of SGC. The effects of pressure and temperature on apparent retention factors of solutes with various polarities were investigated using diol-PEI-HMDS silica particles in SGC.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 89
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 559-564 
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography ; dead time ; multiparametric least-squares adjustment ; homologous series ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In reversed phase liquid chromatography (RP-HPLC), the validity of a multiparametric non-linear least-squares regression iterative method for the determination of the column dead time tM and the regression parameter (slope b), based on the use of alkan-2-ones, alkyl aryl ketones, and 1-nitroalkanes has been evaluated. The determination of tM and b has been extensively studied for two mobile phase systems acetonitrile-water and methanol-water on seven octadecyl-C18 and one octyl C8 analytical columns. The calculated tM and b values were compared with those obtained by Guardino's and Grobler's methods. The influence exerted thereon by the nature of the homologous series, the mobile phase composition, and the packing materials were investigated.
    Zusätzliches Material: 5 Tab.
    Materialart: Digitale Medien
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  • 90
    ISSN: 0935-6304
    Schlagwort(e): SFE ; experimental design ; additives ; recycling ; polyolefins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The performance and feasibility of supercritical fluid extraction (SFE) applied to the extraction of some antioxidants (Irganox 1076, Irgafos 168) and one UV-stabilizer (Chimassorb 81) from both virgin and recycled low density polyethylene (LDPE), and virgin high density polyethylene (HDPE) are studied. Due to the high number of variables a full-factorial design has been applied to minimize the number of experiments required to reach the optimum extraction conditions. Further analysis has been carried out off-line by reversed-phase HPLC. Modification of the physical properties of the polymeric matrix and increased number of recycling cycles as well as the influence of physical properties on the efficiency of SFE are also discussed.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 91
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 595-598 
    ISSN: 0935-6304
    Schlagwort(e): Xylitol ; samarium ; weak association ; equilibrium constant ; capillary electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 92
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 599-603 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; retention ; mixed stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Most commercially available instruments for capillary electrochromatography (CEC) have a fixed configuration and lack the flexibility to use shorter columns. Applying a blended stationary phase (a phase consisting of a given ratio of bare silica and reversed phase material) can simulate columns of different length in CEC. The goal of this work was to examine the effect of the degree of blending of reversed-phase columns (with bare silica) on the speed of the separation of neutral compounds in CEC. Optimum column packing mixture was determined from the variation of the solute retention factors as a function of the ratios of blending of reversed-phase and bare silica. By adjusting the column composition, solute retention factors and the analysis run time were halved when compared to a pure reversed-phase column of the same length. Stationary phase blending can be considered as an additional parameter to mobile phase variation, column temperature and applied electric field for the optimization of selectivity and analysis time. By adjusting the stationary phase composition, mobile phase composition, column temperature and applied electric field, the analysis run time of neutral components was decreased more than 75% when compared to a separation obtained on neat reversed-phase column of the same dimensions. The linear dependence of the retention factors as a function of the blend ratio (reversed phase/bare silica) offers a framework for designing a “blended” packed capillary column for CEC separations.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 93
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography ; retention index ; multiparametric least-squares adjustment ; homologous series ; nitramines ; nitroaromatics ; aminoaromatics and nitrophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In reversed phase liquid chromatography, the retention indices of some neutral and acidic explosives and related compounds (nitramines, nitroaromatics, aminoaromatics, and nitrophenols) based on the alkan-2-one, alkyl aryl ketone, and 1-nitroalkane retention index standards have been determined by the application of a new mathematical adaptation method, viz. a multiparametric least-squares regression iterative method. This method was applied to two types of columns. The first group includes six octadecyl-C18 columns with different packing materials and obtained from different manufacturers, while the second group comprises one octyl-C8 column. The retention indices have been extensively studied using either methanol-water or methanol-phosphate buffer mobile phase systems. The calculated multiparametric retention indices values were compared with those obtained by Guardino's, Grobler's, and Kovàts' methods. The influences of the concentration of the organic modifier in the mobile phase, aqueous mobile phase pH, and the column packing material on the retention indices of the explosives were also investigated. Good agreement was observed between the retention indices calculated by the use of the four mathematical methods for both neutral and acidic explosives.
    Zusätzliches Material: 4 Tab.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 94
    ISSN: 0935-6304
    Schlagwort(e): Organochlorine compounds ; pesticides ; food analysis ; tomatoes ; GLC-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A method is described for the simultaneous extraction and determination of twenty organochlorine pesticides residues [hexachlorocyclohexane (HCH) isomers (α, β, γ, δ), aldrin, dieldrin, endrin, heptachlor and its epoxide (HE), hexachlorobenzene (HCB), α-endosulfan, o,p′-DDD, p,p′-DDD, o,p′-DDE, p,p′-DDE, o,p′-DDT, p,p′-DDT, dicofol, methoxychlor, and mirex] that were spiked in tomatoes. Samples were extracted with ethyl acetate, and the extract was subjected to a rapid clean-up using a Florisil column. The residues were determined by GLC-ECD using two columns of different polarity. The calibration graph correlation coefficient ranged from 0.9903 to 0.9990. The recoveries ranged from 95 to 99% with relative standard deviation ranging from 0.5 to 14.7% in the concentration range 0.005 to 0.2 μg/g. The limits of detection ranged from 0.004 to 0.05 μg/g and the limits of quantification ranged from 0.005 to 0.174 μg/g.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 95
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 628-630 
    ISSN: 0935-6304
    Schlagwort(e): p-Nitrophenol ; urine ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 96
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 635-638 
    ISSN: 0935-6304
    Schlagwort(e): High resolution gas chromatography ; thermal desorption ; archeological cosmetic powders ; PTV injector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 97
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 666-670 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; mixed packing technique ; electroosmotic flow ; retention mechanism ; fast analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Mixed packing capillary electrochromatography (MP CEC) with the stationary phase comprising a physical mixture of strong cation exchange (SCX) phase and octadecysilyl (ODS) phase was developed. With the existence of a sulfonic acid group on the surface of SCX, not only could the electroosmotic flow (EOF) remain high at low pH, but also the hydrophilicity of the stationary phase was increased greatly, leading to broad adaptable ranges of both pH and organic modifier concentration in the mobile phase. At the same time, with the coexistence of C18 on the surface of ODS, both the retention and the resolution of samples were improved. Accordingly, MP CEC combined the advantages of both SCX and ODS columns. Effects of operation parameters on EOF and the capacity factors of solutes as well as the retention mechanism of such a column were studied systematically. In addition, MP CEC columns were used in the analysis of strong polar solutes as well as for the high speed separation of acidic, basic, and neutral compounds in a single run.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 98
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective capillary gas chromatography ; chiral stationary phase ; chiral recognition mechanism ; cholic acid ; cyclocholates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The suitability of cyclocholates as chiral selectors in gas chromatography has been evaluated. We present the synthesis and characterization of two cyclocholates, viz. 3α,7α-diacetoxycyclo[3]cholate and 3α,7α-diacetoxycylo[4]cholate. Mixtures of these new selectors with polysiloxanes were tested as chiral stationary phases in capillary gas chromatography. Several enantiomer separations of common racemates were achieved with the 3α,7α-diacetoxycyclo[3]cholate at 10% in OV-1701 (w/w). It was shown that column efficiency was strongly dependent on temperature and that enantioselectivity was very sensitive to column conditioning. This chromatographic behavior suggested that cyclocholates were only dispersed in polysiloxane. Thus, it was assumed that chiral discrimination occurred via enantioselective adsorption interactions of enantiomers at the surface of the solid chiral selector dispersed in the polysiloxane matrix OV-1701.
    Zusätzliches Material: 11 Ill.
    Materialart: Digitale Medien
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  • 99
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 683-686 
    ISSN: 0935-6304
    Schlagwort(e): Vacuum gas oils ; packed column chromatography ; n-paraffins ; carbon number distribution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Gas chromatographic methods are of widespread use in the petroleum industry for assessing petroleum and derivatives quality. The feedstocks for catcracking processes are very sensitive to the n-paraffin contents, which can be accurately determined using capillary column chromatography. Nevertheless, packed column chromatography does have potential advantages, viz. sometimes shorter analysis times, lower costs, higher column capacity, for vacuum gas oil analysis. This paper presents a method for such a determination using a Dexsil-300 packed column. The results obtained (n-alkane contents, carbon number distribution) agree fairly well with those obtained on a 30 m × 0.25 mm DB-1 fused silica capillary column.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 100
    ISSN: 0935-6304
    Schlagwort(e): Coupled GPC-GC ; gel permeation chromatography ; on-column interface ; co-solvent trapping ; gas chromatography ; large volume injection ; organophosphorus pesticides ; olive oil ; automation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The robustness of an automated on-line GPC-GC-FPD method for the determination of Organophosphorus (OP) Pesticides in olive oil has been significantly improved, now allowing a routine operation. The original GPC-GC transfer technique employed a loop type interface with an early vapor exit and co-solvent trapping. Shooting, caused by boiling delay and malfunctioning of the solvent vapor exit during the transfer of the 3 mL solvent fraction to the retention gap, resulted in insufficient focusing of the OP-pesticides. In this interfacing concept, the GPC fraction is introduced directly into the carrier gas stream during a certain time interval using the Dualchrom pressure- and flow regulation, resulting in a very stable transfer. The interface now basically corresponds to an on-column interface with flow regulation. Via a Pyrex glass door behind the GC-oven door it can be seen that the liquid flow is broken up into alternating gas-liquid segments by the carrier gas flow during transfer. This avoids shooting in the retention gap and broadens the temperature range for successful transfer. By using a smaller sized GPC column the solvent fraction transferred was reduced to 1.3 mL. Methyl acetate/cyclopentane and the co-solvent n-nonane were selected for their lower boiling points. The modified method is very robust and has been applied to the analysis of 28 different OP-pesticides in olive oil with an overall detection limit of 0.002 mg/kg. Routinely 24 h of unattended operation is possible with a cycle time of 75 min.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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