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  • 1995-1999  (2,361)
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  • Analytical Chemistry and Spectroscopy  (8,441)
  • Bone
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Years
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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Diseases of the colon & rectum 42 (1999), S. 1225-1227 
    ISSN: 1530-0358
    Keywords: Colon cancer ; Adenocarcinoma ; Intramuscular metastasis ; Bone ; Heterotopic ossification ; Soft tissue tumor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract PURPOSE: This report presents a patient who developed severe buttock pain because of an ossified intramuscular metastasis from a sigmoid colon cancer. METHODS: This is a case report and review of the literature for intramuscular metastasis from colon cancer. RESULTS: Computed tomography and magnetic resonance imaging showed a soft-tissue mass with heavy calcification. Histologically, mature compact bone was observed with adenocarcinoma cells dispersed among the bony trabeculae. CONCLUSION: When an intramuscular mass is seen, even if it contains extensive calcification, metastasis from colon cancer should be included in differential diagnosis.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Skeletal radiology 28 (1999), S. 90-95 
    ISSN: 1432-2161
    Keywords: Key words DXA ; Bone ; Cadaver ; Biomechanics ; Metastases ; Fracture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract  Objective. To determine whether the load-bearing capacity of human proximal femora with metastatic defects can be predicted from the bone mineral content. Design. The bone mineral content (BMC) of the total proximal femur was measured by dual-energy X-ray absorptiometry (DXA). The femurs were loaded so as to simulate stair ascent or external rotation. Patients. Simulated lytic defects were created using specialized cutting tools in the intertrochanteric region of 32 human cadaveric femora. Bone density measurements were made before and after creating defects. Results. A linear relation could be used to predict failure load from BMC or bone mineral density. The slope of the linear relation was greater for loads representing external rotation than for loads representing stair ascent. The linear relations suggest that the BMC measurements account for both the density of the host bone and the amount of bone removed by the defect. Conclusions. The data suggest that between 70% and 80% of the variation in failure load of human femora with lytic metastatic defects can be predicted from the BMC and that relations between BMC and failure load are sensitive to the type of loading. Combined with information on the loads associated with the activities of daily living, these data may be used to help identify patients in whom prophylactic stabilization might prevent a pathologic fracture.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Mund-, Kiefer- und Gesichtschirurgie 3 (1999), S. 140-145 
    ISSN: 1434-3940
    Keywords: Schlüsselwörter Konfokale Laser-Scanning-Mikroskopie ; Dunkelfeldmikroskopie ; Bisbenzimidmarkierung ; Knochen ; Strahlenfolgen ; Radiogener Osteozytentod ; Key words Confocal laser scanning microscopy ; Microscopy ; Bisbenzimide labelling ; Bone ; Radiation effects ; Osteocytes ; Osteoradionecrosis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Early radiation effects on human bone may lead to osteoradionecrosis (ORN). Direct bone cellular lesions [28] as well as fibrous degeneration of blood vessels [21] are considered to be pathologically relevant. Only few data on initial subclinical radiation effects are available. Patients were grouped according to the dose of radiation and clinical findings. Group 1: sound human bone of lower jaw, mostly collected during orthodontic surgery (n = 10 patients); group 2: specimens of lower jaw from patients with ORN (n = 12 patients); group 3: specimens of lower jaw from patients with head and neck cancer who were preoperatively treated with 36 Gy radiation; group 4: specimens of lower jaw from patients with head and neck cancer (n = 9) who were treated with 60–70 Gy radiation. Specimens were studied by confocal laser scanning microscopy (CLSM), by conventional light microscopy (DL) and by flourescence darkfield microscopy (DFM) after bisbenzimide staining (H 33258) of the viable cellular nuclei. For the correlating study of identical areas in CLSM and DL the specimens were prepared according to the sawing and grinding technique [8]. All the radiated bony specimens, regardless of the dose of radiation, showed areas of extensive or total loss of vitality of the osteocytes. This finding was also evident after 36 Gy and a short interval between radiation and sample collection (group 3). Additionally, in CLSM micromorphologic lesions of the lamellate structure were seen. With these results we can confirm the loss of vitality of the osteocytes as an initial radiation effect as described earlier [10, 23, 28]. In addition to these findings, alteration of the lamellate microstructure was found in the early phase after radiation. The functional and mechanical significance of these findings should be the subject of further studies.
    Notes: Für die infizierte Osteoradionekrose (IORN) des Kiefers werden unterschiedliche pathogenetische Mechanismen initialer Strahlenfolgen im Knochen diskutiert: Wichtige Parameter sind dabei die direkte Zellschädigung der Osteozyten [28] und die Gefäßfibrosierung [21]. Bislang liegen wenige Kenntnisse zum Ausmaß der initialen, subklinischen Veränderungen vor. 4 Probengruppen wurden anhand verschiedener Patientenkollektive definiert: Gruppe 1: gesunde Unterkieferproben meist von orthodontischen Operationen (n = 10 Patienten); Gruppe 2: Unterkieferproben mit manifester IORN (n = 12 Patienten); Grruppe 3: Unterkieferproben nach 36 Gy präoperativer Radio(chemo)therapie (n = 9 Patienten); Gruppe 4: Unterkieferproben nach 60–70 Gy Bestrahlung ohne Hinweise auf IORN (n = 9 Patienten). Alle Proben wurden histotomographisch mit konfokaler Laser-Scanning-Mikroskopie (CLSM), durchlichtmikroskopisch (DL) und dunkelfeldmikroskopisch (DFM) nach Fluoreszenzmarkierung des intakten Zellkerns (Bisbenzimid H 33258) untersucht. Korrelierende Histologien identischer Probenareale erfolgten an Trenndünnschliffen [8]. Als Ergebnisse wurden gefunden: 1. Alle unterschiedlich bestrahlte Knochenproben zeigten Areale mit weitgehendem bis vollständigem Verlust vitaler Osteozyten. Diese Strahlenfolge trat auch schon nach 36 Gy und kurzem Intervall bis zur Operation (Gruppe 3) auf. 2. Im CLSM zeigten sich zusätzlich mikromorphologische Veränderungen der lamellären Struktur, die zwischen den Probengruppen progredient waren. Hieraus können folgende Schlußfolgerungen gezogen werden: 1. Der vorbeschriebene Vitalitätsverlust der Osteozyten [10, 23, 28] konnte als sehr frühe, initiale, radiogene Läsion bestätigt werden. 2. Zusätzlich zeigten sich Veränderungen der lamellären Mikroarchitektur des Knochens als frühe und im Gruppenvergleich progrediente Strahlenläsion. Die mikromechanisch funktionelle Bedeutung dieser Veränderung muß in weiterführenden Untersuchungen eruiert werden.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    European journal of orthopaedic surgery & traumatology 9 (1999), S. 251-254 
    ISSN: 1432-1068
    Keywords: Bone ; Scintigraphy ; symptomatic ; Knee ; Arthroplasty ; Os ; Scintigraphie ; Genou ; Arthroplastie ; Symptomatique
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Résumé Objectif: Evaluation de la scintigraphie osseuse dans l'arthroplastie totale de genou douloureux. Lieu: Hôpital universitaire, Maastricht et Hôpital Maasland, Sittard. Projet: Investigation clinique retrospective. Méthode: Les dossiers cliniques de 27 patients ayant subi une scintigraphie de l'os, ont été étudiés afin d'analyser les plaintes et la façon de décider le diagnostic. Ces patients avaient des symptômes persistants après l'arthroplastie totale du genou. En plus ont été étudiées les radiographies conventionelles et les scanographies isotopes, sans connaître les dossiers cliniques. Sur la base de ces données nous avons évalué les cas dans lesquels la scanographie isotope du genou a contribué de façon décisive au traitement future. Résultats: La scanographie isotope ne contribue pas à la planification du traitement, si l'examen physique ou les radiographies conventionelles n'ont pas apporté de diagnostic clinique. Il s'agissait ici de 37 % des patients de cette série. Dans les cas où le diagnostic clinique était fait, la scanographie isotope a influencé la décision de diagnostic de 65 % des patients. Cependant, pour les autres patients avec diagnostic clinique (35 %), ce ne fut pas le cas. Conclusion : La répresentation radionucléide est de valeur limitée dans le diagnostic d'une arthroplastie symptomatique totale du genou. Elle peut supporter ou rejeter un diagnostic clinique mais entraînera rarement un changement de traitement, dans l'absence de constatations anormales pendant les examens physiques ou radiologiques.
    Notes: Summary Objective: Determination of the value of bone scanning in symptomatic total knee arthroplasties. Setting Academic Hospital Maastricht and Maasland Hospital Sittard. Design: Retrospective clinical investigation. Method: The clinical reports of 27 patients, who underwent a bone scintigraphic study, were investigated for complaints and analysis of diagnostic decision making. These patients had persistent symptoms after total knee arthroplasty. In addition, conventional radiographs and the isotope scans were studied without knowledge of the clinical records. Based on these data we evaluated in which cases isotope scanning of the knee had contributed decisively to the further treatment. Results: Isotope scanning did not contribute to the treatment planning if physical examination or conventional radiographs had not led to a clinical diagnosis. This comprised 37% of the patients in our series. If a clinical diagnosis was present, isotope scanning did influence decision making in 65% of the patients. However in the remaining patients with a clinical diagnosis (35%) this was not the case. Conclusion: Radionuclide imaging is of limited value in the diagnostic process of symptomatic total knee arthroplasty. It may support or reject a clinical diagnosis, but in the absence of abnormal findings at physical examinations or radiologic studies, it seldom will induce a change in treatment
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    European journal of orthopaedic surgery & traumatology 9 (1999), S. 161-165 
    ISSN: 1432-1068
    Keywords: Bone ; Bone substitutes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Biocompatible calcium phosphate ceramics has been used for several years in orthopeadic surgery. We have been using two new synthetic biphasic calcium phosphate ceramics (BCP) since September 1996 for bone defect filling in any orthopaedic or trauma operation where autograft use was not possible or even wanted. The first, Eurocer 400® has 300 to 500 micron wide macropores with a totally interconnected porosity. This salt seed like product can be used in bone defect filling, when solidity is not a major concern. The second, Eurocer 200® has not totally interconnected 200 micron large pores. Its main characteristic is a mechanical resistance up to 30 Mpa. We use it in any case of weight-bearing surgery. Different sizes and presentation forms are available and will be chosen according to the recipient site shape. We report one hundred and fifty cases with a six to thirty month follow-up. In one third of the patients hip revision surgery was addressed. Another third concerned recent trauma or sequelae cases,.whereas the last third involved cold orthopaedic procedures. General principles are the need of a living and non-infected site after thorough debridement if necessary. Osteocompatibility of calcium phosphate ceramic is confirmed by our results. We report no mechanical failure. In all cases X-rays show a progressive integration, with new bone formation. Our substitutes have been histologically studied in nine cases, four to fifteen months after implantation. New bone formation around and in the substitute is impressive. Indeed, their good mechanical properties without loss of biological quality is the most relevant feature of these BCPs, leading to a wider indication field; therefore we have now abandoned the use of any bony auto, allo or xenograft.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 1433-7347
    Keywords: Key words Anterior cruciate ; ligament reconstruction ; Bone ; tunnel enlargement ; Hamstring ; tendons ; Magnetic resonance ; imaging ; Radiographic evaluation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine , Sports Science
    Notes: Abstract The aim of this study was to describe the contrast-enhanced magnetic resonance imaging (MRI) appearance of bone tunnel enlargement detected on radiography after anterior cruciate ligament (ACL) reconstruction with semitendinosus and gracilis tendon endobutton (STG-endobutton) fixation technique. Fourteen patients with a STG-endobutton ACL reconstruction were examined 3 months (n = 1), 1 year (n = 1) and 2 years (n = 12) postoperatively. An age- and sex-matched group with a bone–patellar tendon–bone (BTB) autograft ACL reconstruction with similar follow-up was taken as control. Data on clinical examination, laxity and isokinetic muscle torque measurements, anteroposterior and lateral view radiography were obtained, and knee scores (Lysholm and Tegner) were collected. Contrast-enhanced MRI was performed in the STG-endobutton group with a 1.5-T imager. There were no statistical differences between the groups with respect to clinical findings, stability tests, or knee scores. In the STG-endobutton group the average femoral and tibial bone tunnel diameter detected on anteroposterior view radiography had increased at 2-year follow-up by 33% and 23%, respectively. On MRI the ligamentous graft itself was not enhanced by the contrast medium whereas periligamentous tissue within and around the STG graft bundles showed mild contrast enhancement. In conclusion, the MRI results suggest that enhancing periligamentous tissue accumulated in and around the STG graft associated with the tunnel expansion. In spite of the significant bone tunnel enlargement observed on the follow-up radiography the STG-endobutton knees were stable and the patients satisfied.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1432-5233
    Keywords: Key words Non-enzymatic glycosylation ; Advanced glycation endproducts ; Receptor for advanced glycation endproducts ; Diabetes mellitus ; Osteoblasts ; Bone ; Osteopenia
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Advanced glycation endproducts have been implicated in the development of diabetic complications. In addition, these products could also mediate certain bone alterations such as diabetic osteopenia. Several receptors specific for advanced glycation endproduct-modified proteins have been characterized in different cell types, contributing to the recognition and degradation of senescent proteins. In the present report, we investigated the possible presence of advanced glycation endproduct-binding proteins on osteoblast-like cells. Both UMR106 and MC3T3E1 cell lines express specific advanced glycation endproduct-binding sites, with an affinity constant between 0.4 and 1.7 · 106 M−1, depending on the stage of osteoblastic differentiation; and with a receptor capacity of 1.5–2.0 · 107 sites/cell. Osteoblast-like cells were also found to participate both in the uptake and degradation of advanced glycation endproduct-modified bovine serum albumin at 37°C. Radiolabelled ligand blotting studies confirmed the presence of several membrane binding proteins, with apparent molecular masses of 50, 45–40, 30, 25 and 18 kDa; the major bands corresponded to 30 and 25 kDa proteins. This study provides evidence of the presence of advanced glycation endproduct-specific binding sites, and for their regulation with the stage of differentiation, in two osteoblast-like cells in culture.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    European journal of trauma 25 (1999), S. 230-236 
    ISSN: 1615-3146
    Keywords: Aneurysmatische Knochenzyste ; Knochentumor ; Hand ; Aneurysmal bone cyst ; Bone ; Hand
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Abstract The aneurysmal bone cyst localizised at the longfingers of the hand is an extremely rare clinical entity, particularly considering the age and the distinct aggressiveness in our case. In this specific case of a 53-year-old male the differentialdiagnosis as well as problems of the aneurysmal bone cyst with affection of the phalangeal bone will be discussed. Furthermore the various possibilities of therapy will be focussed on. At first the patient was treated with curettage followed by bone grafting. Already 5 months later a local recurrence appeared. The proximal phalangeal bone and the metacarpophalangeal joint V were almost distroyed. Aiming at preservation of a high funcionality of the hand we amputated the 5th finger in the metacarpophalangeal joint.
    Notes: Zusammenfassung Die aneurysmatische Knochenzyste mit Lokalisation an der Hand, insbesondere an den Phalangen, ist ein extrem seltenes Krankheitsbild. Auch das Alter des Patienten und die ausgeprägte Aggressivität unseres Falles sind bemerkenswert. Anhand der Krankengeschichte eines 53jährigen Mannes mit Befall der Grundphalanx des fünften Fingers der rechten Hand werden die Problemstellung bzw. Differentialdiagnose verdeutlicht und die verschiedenen Therapiemöglichkeiten besprochen. In unserem Fall wurde zunächst eine Kürettage mit anschließender Spongiosaaufftüllung durchgeführt. Bereits nach fünf Monaten kam es zu einem aggressiven Rezidiv mit Zerstörung der gesamten Grundphalanx und des Grundgelenks, so daß wir uns schließlich unter Berücksichtigung der bestmöglichen Funktion der Hand für eine Amputation des Kleinfingers entschieden haben.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Reproduktionsmedizin 15 (1999), S. 405-409 
    ISSN: 1434-808X
    Keywords: Schlüsselwörter Estrogenrezeptoren ; Knochen ; Arteriosklerose ; Endometrium ; Zentralnervensystem ; Key words Estrogen receptors ; Bone ; Arteriosclerosis ; Endometrium ; Central nervous system
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Summary Almost each cell in the body is estrogen-receptive. The strength of estrogen influence on organs or organ systems, however, may vary. Thus, estrogen withdrawal may have more or less severe pathophysiological consequences. Recently, the existence of two estrogen receptors has been established (estrogen receptor α and β = ERα and ERβ and several splice variants of these two basic receptor types have been desribed). This, together with our increasing knowledge about tissue-specific enhancer and repressor genes now allows a better understanding of the organ-specific effects of estrogens. In view of gynecological endocrinology, hormone replacement therapy with estrogens is beneficial for most organs in the body (bone, cardiovascular system, CNS). However, pure estrogen therapy may have deleterious effects in the endometrium of the uterus because it may initiate the development of uterine cancer. In the uterus of most species studied so far, no ERβ but only the classical ERα gene has been described. Hence, drug companies have now intensively begun to search for ERβ-specific estrogens. The first, relatively specific, non-steroidal product that addresses primarily the ERβ is the drug raloxifen, which has been recently introduced clinically. However, also some natural phyto-estrogens appear to be ERβ-specific.
    Notes: Zusammenfassung Fast jede Körperzelle ist estrogenrezeptiv. Es gibt allerdings Organe und Organsysteme, die besonders unter dem Einfluß von Estrogenen stehen und die sich bei Estrogenmangel krankhaft verändern können. Die vielfältigen Wirkungen von Estrogenen konnten nicht vollständig verstanden werden, solange die Existenz von nur einem Estrogenrezeptor quasi ein Dogma war. Erst die Klonierung eines zweiten (Estrogenrezeptor β = ERβ) sowie das bessere Verständnis von gewebespezifischen Enhancer- und Repressor-Genen konnten die vielfältigen und z. T. organspezifischen Wirkungen der Estrogene aufklären. Aus der Sicht der gynäkologischen Endokrinologie ist die Hormonersatztherapie mit Estrogenen für fast alle Organe des Körpers (Knochen, Herz-Kreislauf-System, Zentralnervensystem) segensreich. Eine nicht gestagenbegleitete Estrogentherapie kann allerdings verheerende Folgen am Endometrium mit Entwicklung eines Corpus-Karzinoms haben. Da der Uterus praktisch kein ERβ sondern nur den klassischen ERα exprimiert, hat eine intensive Suche nach ERβ-spezifischen Estrogenen begonnen. Ein erstes, halbwegs spezifisches nicht-steroidales Produkt scheint das kürzlich in die Klinik eingeführte Raloxifen zu sein, aber auch einige Phytoestrogene scheinen ERβ-spezifisch zu wirken.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    International journal of legal medicine 112 (1999), S. 195-197 
    ISSN: 1437-1596
    Keywords: Key words Trauma ; Calcification ; Bone ; Embolism ; Autopsy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine , Law
    Notes: Abstract Embolism of bone marrow to the lungs is a quite frequent finding after trauma but transport and deposition of solid bone is rarely seen, which may simply be because pulmonary calcifications are not recognized as bone fragments. We report on three patients with embolism of bone spicules to small lung arteries of about 0.5 mm in diameter which were plentiful in two of the patients on postmortem examination. However, the true nature of the emboli was only recognizable after decalcification of lung tissues. It appears that trauma occurring in a septic bone lesion has the greatest chance to provoke bone embolism. The bone spicules do not usually occlude vessel lumina and thus do not severely disturb the blood circulation in the lungs. The bone fragments become covered by endothelium and can remain recognizable for months or even years.
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  • 11
    Electronic Resource
    Electronic Resource
    Springer
    Annals of biomedical engineering 27 (1999), S. 508-516 
    ISSN: 1573-9686
    Keywords: Angiogenesis ; Artery ; Bone ; Creeping substitution ; Leukocytes ; Osteocytes ; Reperfusion injury ; Trauma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine , Technology
    Notes: Abstract An in vivo model has been developed for chronic observation of the effects of ischemia on cortical bone remodeling and perfused vascularity. Diaphragm occluders were implanted around the right common iliac artery of four rabbits and inflated to produce 10 h of ischemia to the limb. Microcirculation was monitored with intravital microscopy of injected fluorescent microspheres and FITC-Dextran 70 through a bone window, the tibial bone chamber implant (BCI). Bone resorption and apposition in the BCI were indicated with mineralization dyes. Between 2 and 12 h following release of the occluder, secondary ischemia/no-reflow and other evidence of reperfusion injury were observed. Vessel damage was suggested by abnormally high leakage of FITC-D70 from the few vessels perfused during secondary ischemia. In the weeks following occluder release perfused vasculature increased beyond pre-occlusion levels. Net bone resorption reached a maximum when vascularity passed normal levels. In order to further validate the arterial occlusion model for osteonecrosis, techniques for (1) confirming bone death and (2) detecting increased leukocyte adherence to endothelial cells were added. The dead cell stain Ethidium homodimer-1 was used to tag dead osteocytes immediately after occlusion and produced a measure designated “osteonecrosis index.” To detect leukocytes adhering to vessel walls, carboxyfluorescein diacetate, succinimidyl ester was injected at occluder release. An increase in the number of adherent leukocytes was detected. © 1999 Biomedical Engineering Society. PAC99: 8764Rr, 8717-d, 8719Tt
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  • 12
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 11-16 
    ISSN: 0935-6304
    Keywords: Pyrolysis gas chromatography ; microstructure determination ; syndiotactic copolymers ; styrenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 3 Ill.
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  • 13
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 24-28 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; ECD ; Micro-ECD ; GC detector ; organochlorine pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 6 Ill.
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 33-38 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; chiral separation ; negatively charged chiral selectors ; capillary filling methods ; dual systems ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 5 Ill.
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 43-46 
    ISSN: 0935-6304
    Keywords: Green and roasted coffee ; diterpenes ; cafestol ; kahweol ; 16-O-methylcafestol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 6 Ill.
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  • 16
    ISSN: 0935-6304
    Keywords: Ethanol ; mobile phase ; factorial planning ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 177-180 
    ISSN: 0935-6304
    Keywords: Fresh water systems ; burbot ; organotin compounds ; speciation analysis ; GC-AED ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 18
    ISSN: 0935-6304
    Keywords: RP-HPLC ; GC-MS ; trioxanes ; thermolysis products ; quantitative analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 19
    ISSN: 0935-6304
    Keywords: Multidimensional Gas Chromatography ; orthogonal separations ; GC×GC ; comprehensive two-dimensional chromatography ; characterization of gasoline ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In comprehensive two-dimensional gas chromatography (GC×GC), two capillary columns are connected in series through an interface known as a “thermal modulator”. This device transforms effluent from the first capillary column into a series of sharp injection-like chemical pulses suitable for high-speed chromatography on the second column. Dramatic increases in the resolving power, sensitivity, and speed of the gas chromatograph result. This paper describes the development of a robust and reliable thermal modulator for GC×GC.
    Additional Material: 5 Ill.
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 74-78 
    ISSN: 0935-6304
    Keywords: Polypeptides ; subcritical fluid chromatography ; supercritical fluid chromatography ; carbon dioxide ; additives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The effect of mobile phase modifier and additive on the chromatographic properties of various small polypeptides was explored under subcritical conditions. A polymeric column was used to separate various enkephalin analogs, bradykinin, and oxytocin using a carbon dioxide-based mobile phase with either an ethanol or a 2-methoxyethanol modifier. The role of the modifier was found to be secondary to that of the mobile phase additive. As progressively stronger acidic mobile phase additives were used, the peak profiles of the various polypeptides improved and retention decreased. Heptadecafluorooctanesulfonic acid was found to be the most useful additive for these types of solutes under near-critical conditions, while the potassium salt of heptadecafluorooctanesulfonic acid failed to elute any of the polypeptides. At low temperatures, pressure gradients with a carbon dioxide/ethanol/heptadecafluorooctanesulfonic acid ternary mobile phase produced reasonably good peak profiles with the polymeric column.
    Additional Material: 7 Ill.
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  • 21
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 89-92 
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; heptakis(2,3-di-O-methyl-6-O-tert-butyldimethylsilyl)-β-cyclodextrin ; heptakis(2,3-di-O-acetyl-6-O-tert-butyldimethylsilyl)-β-cyclodextrin ; γ(δ)-thionolactones ; olfactometry ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The even numbered γ(δ)-thionolactones (C6-C12) were investigated, using heptakis(2,3-di-O-methyl-6-O-tert-butyldimethylsilyl)- and heptakis(2,3-di-O-acetyl-6-O-tert-butyldimethylsilyl)-β-cyclodextrin as chiral stationary phases in capillary gas chromatography. The odor characteristics of γ(δ)-thionolactone enantiomers were investigated by enantioselective gas chromatography/olfactometry.
    Additional Material: 4 Ill.
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  • 22
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 93-96 
    ISSN: 0935-6304
    Keywords: Capillary GC ; PTV and on-column injectors ; milk fat triglycerides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 1 Ill.
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  • 23
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 217-221 
    ISSN: 0935-6304
    Keywords: HPLC ; UV detection ; linear range ; method validation ; Beer-Lambert law ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Additional Material: 6 Ill.
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  • 24
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 231-234 
    ISSN: 0935-6304
    Keywords: Trace analysis ; air samples ; BTX ; equilibrium-sorptive enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 4 Ill.
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 119-122 
    ISSN: 0935-6304
    Keywords: Fast gas chromatography ; multi-capillary column ; band broadening ; simulation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 26
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 129-130 
    ISSN: 0935-6304
    Keywords: GC-MS ; kava pyrones ; Alpinia zerumbet ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 27
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 135-143 
    ISSN: 0935-6304
    Keywords: Chromatographic separation techniques ; High Performance Liquid Chromatography (HPLC) ; Gel Permeation Chromatography (GPC) ; Supercritical Fluid Chromatography (SFC) ; Capillary HPLC ; Nuclear Magnetic Resonance (NMR) spectroscopy ; hyphenation of chromatography with NMR spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The hyphenation of chromatographic separation techniques with NMR spectroscopy is one of the most powerful and time-saving methods for the separation and structural elucidation of unknown compounds and molecular compositions of mixtures. Most of the routinely used NMR flow-cells have detection volumes between 40-180 μL for conventional separations with analytical columns, and the newest designs employ detection volumes in the order of 200 nL for capillary separations. The low flow rates used in capillary chromatography permit the use of deuterated solvents. Unequivocal structural assignment of unknown chromatographic peaks is possible by two-dimensional stopped-flow capillary HPLC-NMR experiments.
    Additional Material: 14 Ill.
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  • 28
    ISSN: 0935-6304
    Keywords: Conjugated linoleic acid (CLA) ; silver-ion high performance liquid chromatography (Ag+-HPLC) ; cheese ; analysis ; silver-ion chromatography ; tandem-column Ag+-HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A commercial mixture of conjugated linoleic acid (CLA) isomers, reportedly consisting of six components, was recently resolved into 12 peaks attributed to CLA isomers using silver-ion high performance liquid chromatography (Ag+-HPLC). In this study, the coupling of two analytical silver-ion high performance liquid chromatography columns (tandem-column Ag+-HPLC) in series led to the enhanced resolution of CLA isomers. Many CLA isomers were baseline resolved and the pair 18 : 2 8,10 c/t and 18 : 2 7,9 c/t found in cheese products, was resolved for the first time. In this work, a similar commercial CLA mixture was separated into 16 peaks, while CLA isomers from cheese also gave rise to 16 peaks. As expected, the CLA isomers were separated into three geometric groups in the order trans,trans, cis/trans, and cis,cis. Semi-preparative Ag+-HPLC, followed by gas chromatography-mass spectroscopy of the dimethyloxazoline derivatives, was used to confirm the identity of the newly resolved positional CLA isomers. The double bond configuration of CLA isomers was established by gas chromatography-Fourier transform infrared spectroscopy. Two minor t,t CLA isomers found in cheese, presumably 18 : 2 t6t8 and 18 : 2 t13t15, were also separated. The CLA isomeric composition of 16 commercial cheese products was determined.
    Additional Material: 5 Ill.
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  • 29
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 159-163 
    ISSN: 0935-6304
    Keywords: Multi-dimensional chromatography ; LC-GC ; AED ; memory effects ; fossil fuel ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Conventional operation of the GC Atomic Emission Detector (AED) system involves backflushing of the microwave induced plasma (MIP) during the elution of small volumes of solvent from the GC column. When performing multi-dimensional, on-line LC-GC-AED, significantly larger solvent volumes are introduced into the system and must subsequently be removed. Thus solvent venting procedures are required and the backflushing of the plasma must be extended to facilitate solvent but not solute removal. This study demonstrates the significance of memory effects imparted upon the MIP of the AED if solvent venting is incomplete. Comparison of conventional GC-AED and multi-dimensional LC-GC-AED is made with respect to a fossil fuel sample.
    Additional Material: 3 Ill.
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  • 30
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 171-176 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography (MEKC) ; solid phase extraction (SPE) ; phenylurea(s) ; herbicide(s) ; monuron ; linuron ; diuron ; isoproturon ; monolinuron ; drinking water ; environmental water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The present paper describes the application of capillary electrophoresis in the micellar mode to the separation and quantitative determination of five phenylurea herbicides, viz. monuron, linuron, diuron, isoproturon, and monolinuron, in water samples. Using uncoated fused silica capillary and phosphate-borate buffer (pH 7.0) containing SDS, the five pesticides are resolved in less than 15 min and quantitatively determined by an ultraviolet detector at 244 nm. Method optimization and validation parameters are presented. Good linearity and repeatability were observed for all the compounds studied (correlation coefficients 0.999). The feasibility of the method developed was tested by simultaneous determination of these herbicides in environmental and drinking water samples at the minimum residue levels (MRLs) (0.1 μg/L) after solid-phase extraction (SPE) preconcentration procedure.
    Additional Material: 7 Ill.
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  • 31
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 181-182 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; microwave induced emission spectrometry ; speciation ; mercury ; SPME, headspace SPME ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 1 Ill.
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  • 32
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; interfacing ; sample treatment ; serum ; solid-phase extraction ; sulfonamides ; urine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 33
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 191-194 
    ISSN: 0935-6304
    Keywords: TLC/FID ; simple and double migration ; triangle of solvent selectivity ; lipochemical media ; fatty acid esters ; esterification ; transesterification ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 34
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 201-204 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; flame ionization detection ; solvent effects ; aqueous injection ; toluene analysis ; dioxane ; sample preparation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A gas chromatographic method is presented for determining from 1 to 100 μg/mL of 1,4-dioxane in toluene with purities ranging from commercial to high-purity grades. This method relies on extracting 1,4-dioxane from toluene into water. The water extract is analyzed for 1,4-dioxane content by gas chromatography/flame ionization detection and a capillary column coated with a bonded polyethylene glycol stationary phase. Splitless injection is used to achieve a 1 μg/mL detection limit. Purging extracts with nitrogen after an initial analysis is suggested as an extract clean-up procedure and as a means to confirm the identification of 1,4-dioxane. However, for absolute identification of dioxane, gas chromatography/mass spectroscopy should be considered.
    Additional Material: 2 Ill.
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  • 35
    Electronic Resource
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 213-216 
    ISSN: 0935-6304
    Keywords: Average velocity ; characteristic parameters ; flow rate ; high pressure drop ; low pressure drop ; outlet velocity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: When the column pressure drop is high, the average velocity of a carrier gas is proportional to the square root of the outlet velocity and the flow rate. Characteristic velocity, flow rate and pressure - the boundary conditions between low and high pressure drop regions - are introduced. Previously derived equations for average velocity vs. outlet velocity were modified to include the flow rate and to become more suitable for the separate studies of the low and high pressure drop regions.
    Additional Material: 1 Ill.
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  • 36
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 225-230 
    ISSN: 0935-6304
    Keywords: Green tea ; black tea ; composition ; stability ; capillary electrophoresis ; MEKC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 37
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 235-238 
    ISSN: 0935-6304
    Keywords: Cryogenic modulation ; LMCS ; GC×GC ; multidimensional GC ; comprehensive gas chromatography ; petroleum analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 38
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 242-244 
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; 6-O-ethyl-2,3-O-pentyl-β-cyclodextrin ; essential oils ; carboxylic acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 39
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 247-249 
    ISSN: 0935-6304
    Keywords: High performance liquid chromatography-ultraviolet detection (HPLC-UV) ; Amitraz ; cattle dipping bath ; pesticide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 40
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 261-264 
    ISSN: 0935-6304
    Keywords: On-line coupled LC-GC ; normal phase liquid chromatography ; process samples ; oxygenated compounds ; partially concurrent solvent evaporation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Normal phase liquid chromatography-gas chromatography was used with on-column interfacing and partially concurrent solvent evaporation in the analysis of process samples. Samples were taken from reaction mixtures, where the solvent was toluene. The analytes were oxygenated compounds: methyl isobutyrate, methyl methacrylate, methyl α-formyl isobutyrate, and methyl β-formyl isobutyrate. The analytes were transferred from LC to GC using back-flush with a solvent mixture of pentane and diethyl ether. Linearity, repeatability, and transfer efficiency were determined for the method. The method was applied in the determination of the analytes of two different process samples. The results were in good agreement with results obtained by the gas chromatographic method currently in use for the analysis of the process samples.
    Additional Material: 2 Ill.
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  • 41
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 265-270 
    ISSN: 0935-6304
    Keywords: Critical micelle concentration ; cationic surfactant ; capillary electrophoresis ; tetradecyltrimethylammonium bromide ; dodecyltrimethylammonium bromide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The determination of the critical micelle concentration (CMC) of cationic surfactants by capillary electrophoresis was demonstrated. In this study, tetradecyltrimethylammonium bromide (TTAB) and dodecyltrimethylammonium bromide (DoTAB) were selected as cationic surfactants and propazine was chosen as test solute. In the evolution of the effective electrophoretic mobility of propazine as a function of surfactant concentration, a dramatic change in slope at a particular concentration is a good indication of the CMC of this surfactant. The CMC values determined experimentally were further confirmed by a curve-fitting approach. Simulation of the electrophoretic mobility curves as a function of surfactant concentration in both micellar electrokinetic chromatography and capillary zone electrophoresis using cationic surfactants as an electrolyte modifier was performed for propazine, and the intersection of these two mobility curves allowed us to precisely predict the CMC of the surfactant. The CMC values determined for TTAB and DoTAB are 1.6 ± 0.1 and 11.0 ± 0.1 mM, respectively, in the case of an electrolytic solution consisting of 70 mM phosphate buffer at pH 6.0. Moreover, the applicability of the electroosmotic mobility as a parameter for the determination of the CMC was examined.
    Additional Material: 6 Ill.
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  • 42
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 271-275 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; enhanced solvent extraction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A supercritical fluid extraction/enhanced solvent extraction system (SFE/ESE) was used to remove polar and non-polar analytes from various matrices. Extraction of environmental pollutants from soil, additives from low density polyethylene, sulfa drugs from animal tissue, and drug from tablet was performed using both SFE and ESE. Results showed that a single instrumental system can be used to perform both ESE with organic solvents and SFE with carbon dioxide-based fluids. Each method has its own unique advantages and applications. The ability to carry out both solvent extraction and supercritical fluid extraction with one system has obvious economical advantages.
    Additional Material: 5 Ill.
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  • 43
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 279-282 
    ISSN: 0935-6304
    Keywords: Solid phase microextraction (SPME) ; SPME/HPLC interface ; C-8 refocusing unit ; explosives analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 44
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 294-296 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; capillary ; fused silica ; rotenone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
    Additional Material: 3 Ill.
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  • 45
    ISSN: 0935-6304
    Keywords: Deproteinization ; polychlorobiphenyls ; polychlorodibenzo-p-dioxins ; restricted-access reversed-phase packings ; sample preparation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 46
    ISSN: 0935-6304
    Keywords: Mycotoxin ; T2 ; solid phase microextraction ; GC/FID ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 47
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 438-442 
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; micro-HPLC ; preparation of on-column frits ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Existing methods for preparing frits in packed fused silica capillaries as used for electrochromatography and micro HPLC are not applicable to all silica based packing materials and involve a high thermal stress for both the stationary phase and the fused silica tubing including the polyimide coating. A new procedure for the production of such on-column frits under mild conditions by a sol-gel type reaction of polydimethoxysiloxane (PDMOS) is described in this paper. Reaction conditions were established for optimum mechanical stability and high permeability of the frits. Frits produced in this manner showed no noticeable effect on the overall efficiency.
    Additional Material: 1 Ill.
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  • 48
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 443-448 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic capillary chromatography ; temperature programming ; applied voltage programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Temperature and voltage programming modes were utilized to optimize selectivity and increase the eluting rate of strongly retained compounds in micellar electrokinetic chromatography. Separations obtained by applying temperature, voltage, and a simultaneous combination of temperature and voltage gradient in micellar electrokinetic capillary chromatography were compared with separations performed under isothermal and constant voltage conditions. A complete separation of all the constituents of the test mixture was only achieved in the temperature programming run and in a combination of temperature and voltage programming modes. Simultaneous variations of column temperature and applied voltage during a separation run, yielded a 30% reduction in the total analysis time when compared to a temperature gradient alone. Temperature programming and voltage programming modes may be the gradient methods of choice because of the considerable technical difficulties involved in performing linear solvent gradient elution in micellar electrokinetic chromatography.
    Additional Material: 7 Ill.
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  • 49
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    Journal of High Resolution Chromatography 22 (1999), S. 459-464 
    ISSN: 0935-6304
    Keywords: Fast gas chromatography ; gas chromatography ; resistive heating ; organophosphorus pesticides ; PAHs ; triazines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The features of a resistive-heated capillary column for fast temperature-programmed gas chromatography (GC) have been evaluated. Experiments were carried out using a commercial available EZ Flash GC, an assembly which can be used to upgrade existing gas chromatographs. The capillary column is placed inside a metal tube which can be heated, and cooled, much more rapidly than any conventional GC oven. The EZ Flash assembly can generate temperature ramps up to 1200°/min and can be cooled down from 300 to 50°C in 30 s. Samples were injected via a conventional split/splitless injector and transferred to the GC column. The combination of a short column (5 m×0.25 mm i. d.), a high gas flow rate (up to 10 mL/min), and fast temperature programmes typically decreased analysis times from 30 min to about 2.5 min. Both the split and splitless injection mode could be used. With n-alkanes as test analytes, the standard deviations of the retention times with respect to the peak width were less than 15% (n = 7). First results on RSDs of peak areas of less than 3% for all but one n-alkane indicate that the technique can also be used for quantification. The combined use of a short GC column and fast temperature gradients does cause some loss of separation efficiency, but the approach is ideally suited for fast screening as illustrated for polycyclic aromatic hydrocarbons, organophosphorus pesticides, and triazine herbicides as test compounds. Total analysis times - which included injection, separation, and equilibration to initial conditions - were typically less than 3 min.
    Additional Material: 7 Ill.
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  • 50
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 465-468 
    ISSN: 0935-6304
    Keywords: Amino acid ; stable isotope ; GC-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In order to study protein digestibility by means of noninvasive tracer techniques (stable isotopes), a representative oral tracer, i.e. a stable isotope labeled protein, is needed. Therefore, egg white containing L-[ring-2H5]phenylalanine and L-[ring-2H4]tyrosine was prepared. The aim of this study was to measure the isotopic enrichment of the labeled amino acids in the egg white. The use of a standard GC-MS, based on ion trap technology was found to be a reliable technique. The enrichment of L-[ring-2H5]phenylalanine and L-[ring-2H4]tyrosine, expressed in Molar Percent (MP) amounted to 23.2 MP and 2.8 MP respectively.
    Additional Material: 4 Ill.
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  • 51
    ISSN: 0935-6304
    Keywords: Adhesives ; GC/MS ; headspace analysis ; poly(vinyl acetate) ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 52
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 483-486 
    ISSN: 0935-6304
    Keywords: HPLC ; alumina ; evaporative light-scattering detection ; non-polar lipids ; wax esters ; sterol esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This study describes the performance and capacity of alumina as stationary phase in an HPLC-ELSD (evaporative light-scattering detection) method optimized for the separation of the non-polar lipid classes hydrocarbons, wax esters, sterol esters, triacylglycerols, and sterols, including quantitative determination of these lipid classes in natural samples. By using gradient elution and constant equilibration times between injections, highly reproducible separations of triacontane, stearyl oleate, and cholesterol oleate were accomplished with a binary mobile phase system. Phase A contained 0.5% tetrahydrofuran in hexane and phase B 20% isopropanol and 20% tetrahydrofuran in hexane. The same system was also used to determine the non-polar lipid classes in a zooplankton sample, the major lipid class being wax esters, followed by triacylglycerols, sterol esters, sterols, and hydrocarbons. Substantial amounts of an unknown compound, possibly acylated glyceryl ethers, were also found. The equilibration time of alumina was relatively slow compared to a polyvinyl alcohol stationary phase used earlier by the authors and calibration curves for different lipid classes were more uniform and linear with alumina.
    Additional Material: 4 Ill.
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  • 53
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 495-500 
    ISSN: 0935-6304
    Keywords: CZE ; mobility ratio ; migration time prediction ; mathematical model ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The electrophoretic mobility ratio (R value) of any two ions is constant and independent of the capillary type and electrophoretic conditions if their electrical charges and hydration radii are constant. The use of strong acid salts and quaternary ammonium salts is therefore proposed for the determination of R values. Such analytes are called markers. The following determinations can be carried out: (i) the determination of the migration time corresponding to the electroosmotic flow (EOF) in any capillary under any electrophoretic condition by measuring the migration times of two markers in the condition studied (useful when the EOF is weak); (ii) the determination of the migration time of an analyte in any capillary by knowing the migration time of the markers in the capillary studied. If the pH is changed and the ionization of the analyte is pH dependent, the resulting migration time for the analyte can be calculated. The constancy of the mobility ratios of seven markers was checked experimentally at eight different pH values (between pH 3 and 10), at three temperatures, and for two buffer concentrations. The predicted and experimental migration times were also compared in two different types of capillaries.
    Additional Material: 2 Ill.
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  • 54
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 509-513 
    ISSN: 0935-6304
    Keywords: Fast GC ; fast temperature programming ; resistive heating techniques ; short columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---One possible way to speed up a gas chromatographic analysis is the application of fast temperature programming by using resistive heating techniques. With this heating technique programming rates up to 20° per second can be reached. A relative standard deviation of retention times better than 0.2% is obtained. Using fast temperature programming the analysis-times of a mineral oil sample, an industrial oligomer sample, and toxic compounds in diesel fuel have been reduced 5 to 20 times, compared to a standard temperature programmed analysis. In most cases resistive heating cannot be applied to reduce the analysis time of a complex sample. The use of fast temperature programming is preferable to the use of short columns and columns operated at above-optimum carrier gas velocities.
    Additional Material: 6 Ill.
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  • 55
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 521-526 
    ISSN: 0935-6304
    Keywords: Multichannel silicone trap ; water analysis ; flow rate ; methanol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of Multichannel Silicone Rubber Traps for the direct analysis of organic compounds in water was studied. The optimum collection flow rate for a 10 mL sample was found to be ca. 150 μL·min-1. The effect of methanol on the retention power of the trap was evaluated. The addition of a methanol fraction of up to 40% to the water standards did not show any loss in collection efficiency. It was shown that the extraction of organic compounds from water with the multichannel trap is uncomplicated, i. e. methanol is not required to achieve accurate analyses, concentration of the sample onto the trap is by gravity flow, and excess water remaining in the multichannel trap after water extraction is removed by centrifugation. With the use of the multichannel silicone rubber trap a wide boiling point range of compounds were analyzed from aqueous samples at levels of 1-4 μg·L-1.
    Additional Material: 5 Ill.
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  • 56
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 533-540 
    ISSN: 0935-6304
    Keywords: Chlorobiphenyl congeners ; Aroclor 1254 ; DB-XLB phase ; GC-MS-SIM ; PCB 126 ; toxic equivalency ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Complete PCB congener distributions in a panel of Aroclor mixtures were previously obtained by combining data from several HRGC systems. In that study quantitation of minor components may have been unreliable due to single level calibration against high levels of individual congener standards. Two lots of Aroclor 1254 had markedly different congener distributions. In this study, the design and performance of a congener-specific PCB analysis method employing GC-MS-SIM detection of congeners separated on a DB-XLB capillary column are discussed. Quantitation is carried out against a 6-level inclusive standard curve of a mixture of 144 congeners found in Aroclors. A separate procedure to measure trace levels of PCB 126 in Aroclors using the same system, combined with levels initially acquired for other congeners, facilitates estimation of TEQ values (Toxic Equivalencies of the PCB mixtures to 2,3,7,8-TCDD). PCB congener profiles of 15 Aroclor 1254 mixtures are presented. These profiles show that the less common, high TEQ variety of Aroclor 1254 was manufactured by an atypical, two-stage chlorination process that was apparently used during the final 1% of Aroclor 1254 production (ca. 1974-1976).
    Additional Material: 5 Tab.
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  • 57
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 547-552 
    ISSN: 0935-6304
    Keywords: Water analysis ; polar pollutants ; solid-phase extraction ; chemically-modified polymeric resins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 3 Ill.
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  • 58
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    Journal of High Resolution Chromatography 22 (1999), S. 421-423 
    ISSN: 0935-6304
    Keywords: 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
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 59
    ISSN: 0935-6304
    Keywords: HPLC ; nitrotyrosine ; nitrotocopherol ; analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 9 Ill.
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  • 60
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 449-453 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; experimental design ; cyclodextrin ; chiral separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 5 Ill.
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  • 61
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    Journal of High Resolution Chromatography 22 (1999), S. 454-458 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; reversed phase ; prototypical substances ; retention parameter model ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A set of four prototypical substances (naphthalene, acetanilide, phenol, and benzonitrile) is selected from 26 different analytes used by Seibert and Poole for characterization of the retention behavior of 20 liquid chromatographic systems of a C18 reversed phase with methanol/water and acetonitrile/water as mobile phases. Retention data of 22 different analytes can be calculated from the retention data of the set of prototypical substances with a mean standard deviation of 5.4%. Two phase system maps similar to that suggested by Poole et al. are provided for an octadecylsiloxane-bonded silica sorbent with methanol and acetonitrile as cosolvents with water.
    Additional Material: 2 Ill.
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  • 62
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 475-476 
    ISSN: 0935-6304
    Keywords: Organic peroxides ; gas chromatography ; FID ; cold on-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 1 Ill.
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  • 63
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    Journal of High Resolution Chromatography 22 (1999), S. 469-474 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; SFE modifiers ; pseudoephedrine ; suphedrine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The effect of modifier and additive composition upon pseudoephedrine recovery from spiked-sand and Suphedrine tablets was examined. Recovery was shown to be dependent on CO2 density as well as on the addition of an ion pairing agent to the matrix. The presence of methanol in the extraction vessel prior to SFE was shown to play a significant role in the ion-pair extraction process. Recovery was also shown to be a function of ion-pairing reagent composition and concentration. The most successful recovery was obtained in the presence of 1-heptanesulfonic acid (HSA), sodium salt in methanol at a 5:1 molar ratio (reagent to drug). The increased extractability in the presence of ion-pairing reagent was attributed to reduced analyte polarity and analyte-matrix displacement. Alternatively, a matrix-spiked mixture of methanol and 1% water by itself was just as effective as a matrix-spiked mixture of methanol and HSA for attaining efficient extraction. Several in-cell (e. g. to the matrix) and in-line (e. g. to the fluid) modifiers were examined for the extraction of pseudoephedrine from Suphedrine tablets. The greatest pseudoephedrine recovery from Suphedrine tablets of 82% (7.0%) was achieved with 10% (l% H2O) methanol-modified CO2 in the presence of 400 μL of methanol (l% H2O). Finally AgCl tests and infrared analyses were performed on two tablet extracts. It was confirmed that even in the absence of any in-cell modifier, a small fraction of pseudoephedrine hydrochloride could be extracted.
    Additional Material: 5 Ill.
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  • 64
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    Journal of High Resolution Chromatography 22 (1999), S. 487-489 
    ISSN: 0935-6304
    Keywords: Carboxymethyl derivatives of amines ; dodecyl-L-hydroxyproline ; chelate ring ; chemiluminescence ; ruthenium complex ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Carboxymethyl derivatives of amines containing a chiral α-carbon were separated into enantiomers by high-performance liquid chromatography using octadecylsilanized silica gel coated with N-n-dodecyl-L-hydroxyproline as the stationary phase and an aqueous solution containing copper(II) as the mobile phase. Detection was by post-column reaction involving derivatization to tertiary amine and chemiluminescence reaction of ruthenium bipyridine complex.
    Additional Material: 3 Ill.
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  • 65
    ISSN: 0935-6304
    Keywords: Large volume injection ; packed capillary LC ; temperature programming ; retinyl esters ; vitamin A ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 2 Ill.
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  • 66
    ISSN: 0935-6304
    Keywords: A,C- and A,D-bridged calix[6]arene ; stationary phase ; capillary gas chromatography ; geometric and positional isomer separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A,C-Bridged (ACCX) and A,D-bridged isopropyldimethylsilylcalix[6]arene (ADCX) dissolved in OV-1701 were used as stationary phases in isothermal capillary gas chromatographic separation of some positional isomers. Retention factors and separation factors for the isomers were measured. The isomers investigated are well resolved on the two phases. Retention of all the solutes investigated is longer on ACCX than on ADCX. The longer retention on A,C-bridged calix[6]arene is probably due to extra inductive interactions of the solute molecule with the carbonyl moieties in the phase. Separation factors for closely eluting isomer pairs are similar on the two phases. This seems to indicate that the carbonyl moieties do not play an appreciable role in discriminating the isomer molecules on entering the cavity of the calixarene if the solute is retained by the inclusion process.
    Additional Material: 2 Tab.
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  • 67
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    Journal of High Resolution Chromatography 22 (1999), S. 647-665 
    ISSN: 0935-6304
    Keywords: Two-dimensional GC ; statistical method of overlap ; petroleum ; fuels ; enviromental samples ; organochlorine compounds ; flavors ; aromas ; foods ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The writer of this review published in 1978 a three-part article on two-dimensional gas chromatography in the first three issues of this journal [1]. The review was written at a time when capillary column GC was still in its infancy. Commercial columns were (essentially) unavailable and sample introduction into capillary columns was done exclusively in the split mode. Two-dimensional separations were explored in only a few laboratories. The limitations of capillary column technology made this exercise rather difficult. The introduction of fused silica capillary columns in the early eighties drastically changed the landscape in which gas chromatography was practiced. It took the chromatographic community just a few years to convert from packed columns to capillary columns. Instrumentation and accessories specifically designed for capillary column use came onto the market. This writer had great hopes that the revolution in capillary column GC would be mirrored in the development of instrumentation for Two-Dimensional Gas Chromatography. This never materialized. On the contrary, tentative steps taken by a few manufacturers and suppliers of chromatographic equipment fizzled out. It was perhaps the introduction of relatively inexpensive and user friendly GC/MS instrumentation, in combination with nearly indestructible fused silica capillary columns that took away the incentive to develop commercially viable Two-Dimensional Gas Chromatography. Much of the thinking went like this: why insist on good chromatography if mass spectrometry can do the job without the need for complete separation. Some progress in the further development of conventional Two-Dimensional Gas Chromatography has certainly been made over the last 20 years but there has not been a great deal of excitement. Applications have also been relatively sparse and they are limited to just a few areas. Science does not remain static and chromatography is no exception. Progress in gas chromatography is driven by new technology and ideas. Substantial improvements in two-dimensional GC were not forthcoming until Phillips and his research group introduced and implemented an entirely new form of Two-Dimensional Gas Chromatography, called comprehensive two-dimensional GC, or GC×GC. This breakthrough occurred only in 1991 [2]. It does take some time before scientists change attitudes and habits. There is always a time lag between the introduction of new technology and its general acceptance. The public's attitude toward comprehensive Two-Dimensional Gas Chromatography is probably no exception. The number of scientists who are actively pursuing this new branch of gas chromatography is still very small. It is often a single individual who carries the torch. J.B. Phillips' name is synonymous with comprehensive Two-Dimensional Gas Chromatography. He is not only its inventor and proponent but his fertile mind has initiated research in other related areas. Sadly, he passed away shortly before this review was written. This contribution is dedicated to his memory.
    Additional Material: 16 Ill.
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  • 68
    ISSN: 0935-6304
    Keywords: 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
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 6 Ill.
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  • 69
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    Journal of High Resolution Chromatography 22 (1999), S. 29-32 
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; electroosmotic flow ; frit ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The formation of bubbles in capillary electrochromatography (CEC) is well documented: possible origins include Joule heating and variations in EOF velocity on passing from the stationary phase through the frit and into the open tube. Methods for the prevention of bubble formation are discussed which are confirmed by experimental results. Using frit lengths varying from 1 mm to 6 mm it is shown how frit length is directly related to the likelihood of bubble formation and how this is affected by applied voltage. It is shown that the change in applied voltage across a capillary affects the formation of bubbles and also that rebonding octadecylsilane (ODS) onto the silica frit after formation of the frit can minimize the formation of bubbles and how this effects the chromatography. A method is also described for increasing the robustness of silica capillaries using a column coupler along with modifications made to conventional capillary electrophoresis equipment to cater for CEC.
    Additional Material: 4 Ill.
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  • 70
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; CE ; chemical migration ; food contact plastics ; dihydroxybenzenes ; packaging ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A capillary electrophoresis method has been developed to determine 1,2-dihydroxybenzene and 1,3-dihydroxybenzene in the food simulants distilled water, 3% acetic acid, 15% ethanol, and olive oil. Both substances, used as monomers and additives to make food packaging plastics, could be analyzed within 15 min. The 1,4-dihydroxybenzene isomer was unretained and eluted with the electroosmotic flow, and so the CE method can give only a semi-quantitative estimate of this isomer if it is present as a migrant. The analytical recovery for the 1,2- and 1,3-isomers from spiked simulants was good at 87% to 98% except for 1,2-dihydroxybenzene which could only be recovered to the extent of 58% from olive oil. Calibration graphs were linear and the limit of detection for each substance was 0.6 mg/kg, which is well below migration limits for these substances. It is concluded that CE offers a rapid and reliable analysis for the control of migration from plastics intended for food contact which employ 1,2-dihydroxybenzene or 1,3-dihydroxybenzene during manufacture, and offers a screening method for 1,4-dihydroxybenzene migration.
    Additional Material: 4 Ill.
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  • 71
    ISSN: 0935-6304
    Keywords: Programmed temperature vaporization (PTV) ; GC-AED ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Programmed temperature vaporization injection (PTV) coupled to gas chromatography and atomic emission detector (AED) has been studied for large volume injection of gaseous samples. As examples of the effectiveness of the technique, the results of the analysis of a series of headspace samples of foods such as garlic and onion, and of landfill gases are presented. The volumes of gaseous samples reconcentrated varied from a few milliliters up to liters depending on analyte dilution, through focusing onto a sorbent trap, then rapid liberation into the GC-AED system by programmed thermal desorption. Despite the high carrier gas flow rates associated with direct PTV-GC, AED performance and sensitivity were unaffected. The detailed elemental information obtained from the PTV-GC-AED analyses was confirmed using a PTV coupled to a gas chromatograph with ion trap detector mass spectrometer as detector (PTV-GC-ITD/MS).
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  • 72
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 55-58 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic capillary chromatography ; sample dissolving solvent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 73
    ISSN: 0935-6304
    Keywords: Sulfobutyl ether-β-cyclodextrin ; micellar electrokinetic chromatography ; separation of regioisomers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 74
    ISSN: 0935-6304
    Keywords: HPLC ; di(2-ethylhexyl) phthalate ; migration ; foods and food simulants ; PVC cling film ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 75
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 79-82 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; thickeners ; monosaccharides ; PMMA capillaries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Gelling agents based on polysaccharides have become extremely important in the food industry. As more and more products like soups and sauces have become available in lyophilized form, thickeners have to be added to give a controlled consistency to the finished meal. A capillary electrophoretic method has been developed to investigate the monosaccharide composition of hydrolyzed thickeners. 2-Aminoanthracene was used as a derivatization reagent to allow sensitive fluorescence detection. This system was applied to a set of standard thickeners as well as to food samples.
    Additional Material: 5 Ill.
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  • 76
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 83-88 
    ISSN: 0935-6304
    Keywords: Large volume injection ; programmed-temperature vaporizer ; organic acids ; phenols ; derivatization ; trimethylsulfonium hydroxide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The combination of on-line methylation using trimethylsulfonium hydroxide with large volume injection of 100 μL was evaluated for the analysis of organic acids and phenols in water. Solvent split injection was applied with complete evaporation of the solvent before analytes were transferred onto the GC column. Despite complete solvent removal, losses were very low compared to conventional splitless injection even for volatile acidic compounds such as propionic acid and phenol. This is explained by intermediate formation of low volatility trimethylsulfonium salts of the analytes which were held in the injector for long evaporation times of up to 10 min, if the evaporation temperature was as low as 10°C. Using a simple liquid/liquid extraction procedure, volatile fatty acids, dicarboxylic acids, benzoic acids and phenols could be detected in 5 mL of water at concentrations of 0.04-0.1 μmol/L with GC/MS in full scan mode. Lactic, pyruvic, and also malonic acids could only be detected at higher levels because of their limited extractability from water as well as their poorer methylation yields. The method provides an easy way to sensitively detect acidic compounds of medium to high volatility in water. It was applied for screening of organic acids and phenols in batch cultures of anaerobic bacteria of which one example is shown.
    Additional Material: 4 Ill.
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  • 77
    ISSN: 0935-6304
    Keywords: Capillary GC ; milk fat purity ; chemometrics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The adulteration of milk fat with foreign fat has been and still is a major concern in the dairy industry. Milk fat purity is currently evaluated by triglyceride analysis by using the Official EU method. The detection limit of the various vegetable and animal fats ranges between 4 and 6%. This research was carried out to verify whether it is possible to decrease the detection limits of beef tallow, which is the most widely used adulterating animal fat. For this purpose, determinations of diglycerides and 3,5-cholestadiene, together with the Official EU method, were applied both to several samples of pure milk fat and to mixtures of milk fat with different percentages of beef tallow. The best results were obtained combining the data deriving from the three determinations by multivariate statistical techniques; in particular, the statistical model obtained by the UNEQ technique seems to be able to decrease the detection limit of beef tallow from 5.2 to 2%. The diglyceride and 3,5-cholestadiene evaluation, combined with the Official EU method for triglycerides, can be usefully applied both to detect small additions of beef tallow and to demonstrate the adulteration of milk fat samples showing results close to the detection limit of the official method.
    Additional Material: 7 Ill.
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  • 78
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 109-115 
    ISSN: 0935-6304
    Keywords: Solid-phase microextraction ; capillary gas chromatography ; volatile polar compounds ; water matrix ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A method was developed for the analysis of volatile polar compounds in a water matrix using open cap vials Solid Phase Micro-Extraction (SPME) and Capillary Gas Chromatography (CGC). Both SPME techniques - direct sampling and headspace - were tested. Optimization of experimental conditions - exposure time, desorption time, with headspace SPME in addition the influence of the temperature and ionic strength of the sample solution on compound sorption, and finally GC response - were investigated. The analytes were extracted by directly immersing the 85 μm polyacrylate fiber in the aqueous sample or in the headspace. The linear range of the preconcentration process and the precision were examined. The amount of polar analytes sorbed on the fiber was determined and was found to be concentration dependent; it amounted to 0.014-0.64% in the concentration range of 0.00425-425 ppm studied in aqueous solution for direct sampling SPME and to 0.011-2.76% for solutions of concentration 0.0425-255 ppm for headspace SPME. The limits of determination were ascertained. Headspace SPME was applied to the analysis of real-life samples.
    Additional Material: 5 Ill.
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  • 79
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 126-128 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography ; capillary electrophoresis ; amines ; cyclodextrins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 80
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 123-125 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography (GC) ; atomic emission detection (AED) ; human plasma ; drug monitoring ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 81
    ISSN: 0935-6304
    Keywords: RP-HPLC ; theophylline ; asthma ; apnea ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 82
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 153-158 
    ISSN: 0935-6304
    Keywords: Vapor analysis ; nerve agents ; sulfur mustard ; data acquisition ; automation ; valve injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 6 Ill.
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  • 83
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 149-152 
    ISSN: 0935-6304
    Keywords: 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
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 3 Ill.
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  • 84
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 63-66 
    ISSN: 0935-6304
    Keywords: Divinylbenzene copolymers ; exclusion limit ; size exclusion chromatography ; surface area ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 85
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 164-170 
    ISSN: 0935-6304
    Keywords: Food packaging ; functional barrier ; gas chromatography ; laminated paperboard ; mass spectrometry ; single sided headspace ; paperboard ; plastic film ; polymer film ; test cell ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A new cell for single sided headspace sampling has been developed for the analysis of volatile organic compounds from food packaging paperboard and laminated paperboard. The cell, which samples the volatile organic compounds over a selected surface, is useful for determining the barrier function of laminated paperboards with respect to volatile compounds. The analysis of volatile organic compounds is carried out by purge and trap capillary gas chromatography in combination with mass spectrometric detection and compound identification. The new sampling cell was constructed to facilitate specific analysis of organic compounds from only one side of a laminated paperboard. The construction and the operating principles of the new sampling device are described. The repeatability of the single sided headspace procedure was found to be quite good. Relative standard deviations of about 5-7% were obtained for the major compounds quantified in replicate headspace analyses of a laminated paperboard. The volatile compounds released from the inner side of a food packaging paperboard sample with different surface composition on the two sides were determined. The barrier function against volatile organic compounds of some laminated paperboards was investigated employing the new headspace cell.
    Additional Material: 7 Ill.
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  • 86
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 188-190 
    ISSN: 0935-6304
    Keywords: LC stationary phases ; porous graphitic carbon ; surfactant ; alkyl glycosides ; glycosides ; evaporative light scattering detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 87
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 195-200 
    ISSN: 0935-6304
    Keywords: Multi-dimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; GC×GC ; BTEX ; aromatics ; reformulated gasoline ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 1 Ill.
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  • 88
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 205-212 
    ISSN: 0935-6304
    Keywords: Membrane extraction ; hollow fiber membrane ; thermodesorption ; GC-MS ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 10 Ill.
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  • 89
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 222-224 
    ISSN: 0935-6304
    Keywords: High-performance liquid chromatography ; Artemisia capillaris ; phenolic compounds separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 90
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 103-108 
    ISSN: 0935-6304
    Keywords: HPLC ; stationary phase ; copper-amine complex ; aromatic amines ; polyaromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Chromatographic silica (10 μm) was chemically modified with the silylating agent: [3-(2-aminoethyl)aminopropyl]trimethoxysilane (AEAPTS). The reaction product was characterized by elemental analysis and infrared and 13C and 29Si NMR spectra. The chemically modified silica was treated with Cu(II) in methanol medium. This cation was strongly adsorbed through complexation by the pendant ethylenediamine groups attached to the silica surface. The complex formed on the silica surface was shown to be stable in both aqueous and non-aqueous media. The aim of Cu(II) immobilization is to use this new material as a stationary phase in High Performance Liquid Chromatography (HPLC). Separations of synthetic mixtures of aromatic amines and of polyaromatic hydrocarbons were undertaken using 150×3.9 mm HPLC columns packed with the modified silica, with and without copper ions, to follow the influence of the cation on the chromatographic separation and to verify the efficiency of the new stationary phase for HPLC.
    Additional Material: 6 Ill.
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  • 91
    ISSN: 0935-6304
    Keywords: Fast gas chromatography ; peak band broadening ; packed capillary columns ; narrow-bore columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 92
    ISSN: 0935-6304
    Keywords: Tebuthiuron ; GC-MS ; HPLC ; drinking water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 93
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 245-246 
    ISSN: 0935-6304
    Keywords: Chloride ; suppressed ion chromatography ; concrete ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 1 Ill.
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  • 94
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 251-255 
    ISSN: 0935-6304
    Keywords: Multi-dimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; GC × GC ; mass spectrometry ; petroleum ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 4 Ill.
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  • 95
    ISSN: 0935-6304
    Keywords: Molecular imprinting ; PAH ; molecular recognition ; selectivity ; redox polymerization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 4 Ill.
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  • 96
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 276-278 
    ISSN: 0935-6304
    Keywords: Cyclic carbonates ; thermal stability ; chemical stability ; gas phase chromatography ; liquid phase chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 97
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 283-286 
    ISSN: 0935-6304
    Keywords: Evaporative light scattering detection ; capillary nebulizer ; packed capillary ; columns ; high temperature liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 5 Ill.
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  • 98
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 303-304 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; food analysis ; pesticide residues ; thiabendazole ; imazalil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 99
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 305-307 
    ISSN: 0935-6304
    Keywords: High temperature gas chromatography ; chocolate analysis ; triacylglycerols determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 100
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 309-314 
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; isomers ; pneumocandins ; separation ; transition metal ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---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.
    Additional Material: 4 Ill.
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