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  • Electronic Resource  (5,893)
  • 1985-1989  (5,893)
  • Analytical Chemistry and Spectroscopy  (5,836)
  • MRI
  • Nuclear reactions
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  • Electronic Resource  (5,893)
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Year
  • 1
    ISSN: 1279-8517
    Keywords: Cryosection ; MRI ; Cerebellopontine angle ; Microsurgery
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Résumé L'angle ponto-cérébelleux est une région anatomique profondément située à la face antérolatérale du tronc cérébral et dont l'accès est rendu délicat par la présence de pédicules vasculonerveux. L'importance fonctionnelle de ces n. crâniens (trijumeau, facial, vestibulo-cochléaire, glossopharyngien, vague et accessoire) justifie dans certains cas, l'utilisation de voies chirurgicales particulières. En effet, les processus tumoraux, situés entre le paquet acoustico-facial en arrière, et le n. trijumeau en avant, sont d'accès délicat par les voies sous-occipitale et sous-temporale transcanalaire. La tentative de préservation de l'audition dans les situations particulières où le côté contro-latéral à la tumeur n'est plus fonctionnel, justifie l'utilisation d'une voie anatomique sous-temporale transcanalaire élargie par ouverture de la tente du cervelet. L'étude anatomique et chirurgicale expérimentale expose les possibilités de cette voie d'abord.
    Notes: Summary The cerebellopontine angle is an anatomic region situated deeply at the anterolateral aspect of the brainstem, access to which is complicated by the presence of neurovascular bundles. The functional importance of these cranial n. (trigeminal, facial, vestibulo= cochlear, glossopharyngeal, vagus and accessory) calls for the use of special surgical routes of access in certain cases. In particular, tumors situated between the vestibulocochlear-facial bundle behind and the trigeminal n. in front are difficult to reach by the suboccipital and subtemporal transmeatal routes. The endeavor to preserve hearing in particular situations, where the side opposite the tumor is no longer functional, justifies the use of a subtemporal transmeatal route extended by opening the tentorium cerebelli. This anatomic and experimental surgical study deals with the possibilities of this route of approach.
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  • 2
    ISSN: 1279-8517
    Keywords: Biomechanics of CNS ; Cranio-vertebral junction ; Medullo-spinal junction ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Résumé Dans le but d'étudier la mobilité normale de la jonction bulbomédullaire durant la flexionextension de la tête, nous avons exploré en IRM dans le plan sagittal 18 jeunes volontaires. L'appareil Magniscan 0,15 Tesla a été utilisé avec des séquences de spin écho courtes, 16 fois en antenne corps et 2 fois en antenne de surface. Dans les limites de notre méthodologie, le secteur global de mobilité cervico-céphalique varie de 31 à 100° (moyenne 63°), le secteur de mobilité O-C1C2 varie de 4 à 39° (moyenne 19°), le secteur de mobilité bulbomédullaire varie de 1 à 32° (moyenne 14°). Lors de la flexion, l'espace libre diminue 11 fois devant la protubérance, 14 fois devant le bulbe et 11 fois devant la moelle cervicale. La partie basse du V4 s'abaisse dans 4 cas en flexion. Aucune modification de la forme du V4 n'a pu être notée. Bien que cette étude soit critiquable à bien des égards, nous pouvons affirmer: que les variations de l'angle bulbomédullaire dans le plan sagittal durant la flexion-extension de la tête sont effectives; qu'elles sont étroitement corrélées à celles de la charnière cranio-rachidienne; que durant le mouvement de flexion, la jonction bulbomédullaire se déplace en avant.
    Notes: Summary Sagittal sections of the brain-stem made by MRI reveal differences in the angle formed by the medulla and the cord. In order to study the normal mobility of this region of the CNS during flexion and extension of the head, sagittal MRI studies were made in the sagittal plane in 18 young volunteers. The volunteers were in dorsal decubitus with the cervical spine first flexed and then extended, with the movement localized to the cranio-cervical junction as far as possible. T1-weighted sequences were used, with body coils in 16 cases and surface coils in two. Measurements were related to global cranio-cervical range of movement, movement at the craniocervical junction and spino-medullary movement. Variations in the depth of the free space in front of the medulla, pons and spinal cord during movement were also noted. We also checked for downward shift of the lower part of the 4th ventricle and modification of the shape of the ventricle during flexion-extension. The global range of cranio-cervical movement was between 31 and 100° (average 63°). The range between the cranium and C1C2 was 4 to 39° (average 19°) and the spino-medullary range was from 1 to 32° (average 14°). During flexion, the free space narrowed in front of the pons 11 times, in front of the medulla 14 times and in front of the cervical cord 11 times. There was a downward shift of the lower part of the 4th ventricle during flexion in 4 cases but no change in shape was noted. Though this study is open to criticism from several aspects, it may be concluded that variations of the spino-medullary angle in the sagittal plane during flexion-extension do occur, that they are closely correlated with movements at the cranio-cervical junction, and that the spino-medullary junction moves forward during flexion.
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  • 3
    ISSN: 1436-2813
    Keywords: MRI ; pancreatic carcinoma ; vascular involvement
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract A retrospective analysis was made to evaluate the diagnostic accuracy of magnetic resonance (MR) imaging for pancreatic cancer. Twenty-one lesions from 21 patients with pancreatic cancer were examined and all except one, were identified on MR images by a disparity in contrast and/or morphological enlargement. The patients were divided into 3 groups, based on the relationship between the tumor and the portal vein, seen on the MR images. These groups were defined as the separate, touching, and surrounding groups. The MR findings correlated with the findings at laparotomy in 16 patients, 10 of whom underwent tumor excision. In the remaining 4, the MR findings correlated with the angiographic findings. The presence or absence of vascular involvement was correctly diagnosed in 18 of the 21 patients. MR imaging proved useful for detecting pancreatic cancer and cancerous infiltration into the portal vein. MR imaging should therefore aid the surgeon in determining the operability and/or curability of patients with pancreatic cancer.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0942-0940
    Keywords: Subarachnoid haemorrhage ; negative angiography ; MRI ; anterior communicating artery aneurysm
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A case of a ruptured aneurysm is presented in which the angiograms did not disclose the sac. Rupture of an aneurysm of the anterior communicating artery was suspected from the distribution of subarachnoid blood on computerized tomography (CT), and the presence of a sac was highly suggestive on magnetic resonance imaging (MRI), which led us to open surgery. A non-thrombosed aneurysm was discovered at the suspected site, and successfully clipped. The necessity is discussed of MRI investigation in patients with subarachnoid haemorrhage (SAH) of unknown aetiology.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Surgical and radiologic anatomy 11 (1989), S. 141-147 
    ISSN: 1279-8517
    Keywords: MRI ; Cervical spine ; Bachial plexus ; Carpal tunnel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Résumé En raison de la bonne définition anatomique des images obtenues par résonance magnétique nucléaire (IRM), nous avons défini les coupes IRM qui permettent d'étudier les nerfs du membre supérieur
    Notes: Summary In view of the good anatomic definition of the images obtained by magnetic resonance imaging (MRI), we have defined MRI sections allowing study of the nerves of the upper limb.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    Surgical and radiologic anatomy 11 (1989), S. 163-169 
    ISSN: 1279-8517
    Keywords: MRI ; Mandible
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Résumé Dix-huit patients ayant une anomalie de la mandibule et deux volontaires normaux ont été étudiés par IRM. Des corrélations ont été faites avec les données de la TDM, des radiographies simples, de l'examen clinique et des constatations chirurgicales lorsqu'elles étaient disponibles. Dans les tumeurs primitives de la mandibule, l'IRM est capable de différencier les lésions solides et les lésions kystiques. Dans les envahissements secondaires de la mandibule par les tumeurs malignes, l'IRM peut montrer le remplacement du haut signal normal de la moelle osseuse par un bas signal tumoral. Dans certains cas, l'étendue de l'atteinte de la moelle osseuse observée en IRM et confirmée par la chirurgie était significativement sous-estimée par l'examen clinique, les radiographies simples et la TDM. Il ressort de cette expérience limitée que l'IRM peut jouer un rôle important dans l'imagerie des affections de la mandibule.
    Notes: Summary Eighteen patients with abnormalities of the mandible and two normal volunteers were studied with MRI. Correlation was made with MR, CT, plain X-rays, clinical examination, and surgical findings when possible. In primary tumors of the mandible, MR was able to differentiate between solid and cystic lesions. In the cases of secondary invasion of the mandible by malignant tumors, MR was able to demonstrate replacement of the normal high signal bone marrow by low signal tumor. In some cases, the extent of marrow involvement shown on MR and confirmed at surgery was significantly underestimated by clinical examination, plain films, and CT. From this limited experience, it appears that MR may play an important role in imaging pathology of the mandible.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Acta neurochirurgica 96 (1989), S. 15-25 
    ISSN: 0942-0940
    Keywords: Subependymoma ; ependymoma ; polymorphism ; flow-cytometry ; morphometry ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The frequency of asymptomatic subependymomas was 0.4% in 1,000 serial routine necropsies and 0.7% in symptomatic subependymomas from 1,000 serial surgical specimens of intracranial neoplasms. Among patients with subependymoma (7 symptomatic and 4 asymptomatic), we found 3 cases of marked nuclear polymorphism (NP) in biopsy specimens. The subjective NP was objectively quantified by computer-assisted morphometry, by which a significant difference in nuclear size between these three cases and other cases (p 〈 0.005) was revealed. This morphological characteristic correlated with the results of DNA-analysis by flow fluorescence cytometry (FFCM): subependymomas with NP demonstrated higher S and G 2/M phases in a diploid pattern than other benign gliomas of our series. From the clinical data including prognosis, however, no remarkable difference was found between the NP group and other groups. The possible existence of less benign variant should be considered in the diagnosis and treatment of subependymoma.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    Acta neurochirurgica 101 (1989), S. 108-111 
    ISSN: 0942-0940
    Keywords: Epidermoid ; intracranial ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Magnetic resonance imaging (MRI) was performed in five cases of intracranial epidermoid. In three of the five patients, the lowdensity mass on the CT scans showed as low intensity on the T1 and high intensity on the T2 weighted images. In the two other patients, the masses with high or isodensity on CT showed as high intensity on the T1 weighted images and as high or low intensity on the T2 weighted images. Thus, the intensity of epidermoid on MRI correlated fairly well with the CT density, although the former was more variable. The variety of intensities on MRI reflects differences in the chemical composition of the components in the epidermoid tissue in addition to differences in the solid and liquid state of the tissue. An epidermoid could have similar MRI findings as an arachnoid cyst with regard to intensities but its irregular margin provides a useful guide for differentiation. As in other tumours, MRI is superior for evaluation of the size and the extent of the epidermoid as well as the displacement of important neurovascular structures.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 31 (1989), S. 16-18 
    ISSN: 1432-1920
    Keywords: MRI ; Hereditary cerebellar ataxia ; Cerebellum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Thirty-two patients with primary progressive cerebellar ataxia were studied using MRI. This technique is better than CT in demonstrating atrophy of cerebellar structures as well as of brainstem and spinal cord. The differential diagnosis from other diseases particularly with multiple sclerosis is easier. The degree of ataxia correlated well with the degree of atrophy of cerebellum. However we could not see any correlation between the degree of atrophy and the onset and duration of the disease and no certain specific aspects could be demonstrated in the different groups examined.
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  • 10
    ISSN: 1432-1920
    Keywords: Gradient recalled echo ; MRI ; Sinus occlusion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary With T1-weighted gradient recalled echo (GRE) MR images and flow compensation, we studied the superior sagittal sinus in 3 normal volunteers and 3 patients with sinus occlusion. In these images, sites of patency of the superior sagittal sinus were identified due to the high signal intensity of the normal sinus. Tumor invading the sinus was nearly isointense with cerebral gray matter. T1-weighted GRE imaging proves to be an effective technique to evaluate sinus blood flow.
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  • 11
    ISSN: 1432-1920
    Keywords: Nerve root avulsion ; Traumatic meningocele ; CT ; Myelography ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A case of traumatic lumbar meningoceles at four levels in combination with total and partial nerve root avulsion and with perservation of a nerve root is reported. Several diagnostic imaging techniques (myelography, CT, myelo-CT and MRI) are compared and their value in demonstrating the continuity of the nerve roots is discussed. MRI could assess the continuity of a nerve root in a traumatic meningocele, not demonstrable by myelography or myelo-CT. The combination of myelography, myelo-CT and MRI is likely to provide a complete diagnostic evaluation of nerve root lesions.
    Type of Medium: Electronic Resource
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  • 12
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 31 (1989), S. 391-395 
    ISSN: 1432-1920
    Keywords: Brain metastasis ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary For the demonstration of brain metastases both CT and MRI are available as diagnostic modalities. To compare both imaging methods as to their sensitivity in detecting brain metastases CT scans and MR images of 60 patients with suspected brain metastases were evaluated. Comparing contrast-enhanced CT and plain MRI neither modality was found to be clearly superior in this respect.
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  • 13
    ISSN: 1432-1920
    Keywords: Opsoclonus ; Myoclonus ; Cerebellum ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary We report a case of a child with opsoclonus-myoclonus syndrome. Neuroradiological studies indicated a lesion in the cerebellar vermis. A cerebellar biopsy revealed changes consisting of Purkinje and granular cell loss with gliosis. This case report documents the correlation of radiologic and pathological findings in a patient with opsoclonus-myoclonus syndrome.
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  • 14
    ISSN: 1432-1920
    Keywords: AIDS ; Central nervous system ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary We report a series of thirteen patients with nervous system complications out of a total of thirty AIDS patients admitted to our hospital over the last two years for which CT and/or MRI have been performed. Five were homosexual men and eight patients (5 men, 3 women) were of African origin (Zaïre and Rwanda) (n=5) or had had sexual intercourse with the local African population (n=3). The nervous system complications encountered included: toxoplasma gondii brain abscess (2 patients); cryptococcus neoformans meningitis+toxoplasmosis (1 patient); toxoplasmosis+lymphoma (2 patients); progressive multifocal leucoencephalopathy (1 patient); lymphocytic meningitis or encephalitis (3 patients); lymphoma (1 patient); polyradiculoneuritis (3 patients). Three of thirteen patients had multiple intracranial abnormalities: one had concomitant intraparenchymal toxoplasma abscess and cryptococcal meningitis; in one patient a lymphoma developed after the successful medical treatment of a toxoplasma abscess; conversely, one patient developed a toxoplasma abscess two years after mediastinal radiotherapy for a systemic non-Hodgkin lymphoma. In conclusion, in our experience, nervous system toxoplasmosis is the most frequent AIDS related CNS complication. Our series demonstrates the high frequency of a second neurological disease occurring either concomitantly or separately. In these cases, while CT may readily identify the intracranial abnormalities, it contributes little towards an etiological diagnosis. Finally, our series illustrates the importance of a central African endemic focus for AIDS.
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  • 15
    ISSN: 1432-1920
    Keywords: MS ; White matter lesions ; SAE ; MRI ; T1-weighted images
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The aim of the study was to define reliable criteria for the differentiation of MR imaging between patients with MS and with “vascular” white matter lesions/SAE. We examined 35 patients with proven MS according to the Poser criteria and 35 patients with other white matter lesions and/or SAE. The result is that with MR a differentiation can be achieved provided that T1-weighted spin-echo sequences are included and the different pattern of distribution is considered. MS plaques are predominantly located in the subependymal region, vascular white matter lesions are mainly located in the water-shed of the superficial middle cerebral branches and the deep perforating long medullary vessels in the centrum semiovale. Infratentorial lesions are more often seen in MS. Confluence at the lateral ventricles is frequently accompanied by confluent abnormalities around the third ventricle, Sylvian aqueduct, and fourth ventricle, which is uncommon in SAE. In MS many lesions visible on T2-weighted images have a cellular or intracellular composition that renders them visible also on T1-weighted ones as regions with low signal intensity and more or less distinct boundary. “Vascular” white matter lesions and SAE mainly represent demyelination and can there-fore be seen on T2-weighted images, but corresponding low signal intensity lesions on T1-weighted images are uncommon. In some exceptions there are such lesions with low signal representing lacunar infarcts or widened Virchow-Robin-spaces.
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  • 16
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 31 (1989), S. 180-183 
    ISSN: 1432-1920
    Keywords: Craniopharyngioma ; Infrasellar region ; MRI ; CT
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A rare case of infrasellar craniopharyngioma mainly occupying the paranasal sinuses, the infratemporal fossa and the skull base is presented. The patient had been treated by an otolaryngologist as a case of mucocele of the sphenoid and ethmoid sinuses because the biopsy specimens obtained at endonasal surgery failed to confirm the true diagnosis. Computed tomography (CT) showed multilobulated low density cysts in the paranasal sinuses, infratemporal fossa and skull base, and the cyst wall was enhanced. Magnetic resonance Imaging (MRI) revealed the cysts to have high intensity in both T1-and T2-weighted images, and excellent three-dimensional visualization was obtained. Characteristic motor-oil-like fluid was aspirated during transnasal surgery and the diagnosis of craniopharyngioma was confirmed by histological examination.
    Type of Medium: Electronic Resource
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  • 17
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 31 (1989), S. 273-275 
    ISSN: 1432-1920
    Keywords: Epidermoid cyst ; Iatrogenic pathology ; MRI ; Spine ; Myelo-CT
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary An 11-year-old boy, treated for acute lymphatic leukemia at the age of 2 with intrathecal injections of Methotrexate, presented with a two year history of pain and signs of lumbo-sacral lesion. MRI, myelography and myelo-CT demonstrated an intradural L4-L5 epidermoid tumor which was removed. Iatrogenic implantation of epithelial cells at the age of two with lumbar punctures is most likely. Decline in incidence of lumbar iatrogenic epidermoid cysts, now an exceedingly rare event, is probably related to improved needles for lumbar punctures.
    Type of Medium: Electronic Resource
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  • 18
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 31 (1989), S. 349-351 
    ISSN: 1432-1920
    Keywords: Neurocutaneous melanosis ; Lipoma ; Spine ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A case of neurocutaneous melanosis developing a leptomeningeal melanoma is described in a ten year old girl in whom an intraspinal lipoma had been resected seven years earlier. Standard and CT myelographic findings are described and the complementary role of Gadolinium-enhanced MRI is discussed. The literature is reviewed and the association of a lipoma and neurocutaneous melanosis has not been encountered.
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  • 19
    Electronic Resource
    Electronic Resource
    Springer
    Journal of neurology 236 (1989), S. 364-366 
    ISSN: 1432-1459
    Keywords: Marchiafava-Bignami disease ; corpus callosum ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Marchiafava-Bignami disease (MBD) is a rare complication of chronic alcoholism. Most reported cases have been diagnosed at autopsy. With CT and, especially, MRI it is possible to diagnose MBD in its early stages. Lesions of CNS structures other than the typical demyelination of the corpus callosum are described ante mortem in a patient with MBD. The more frequent use of CT and MRI in sudden onset encephalopathies of alcoholics could reveal the real incidence of MBD, and the consequent detection of other involved CNS systems might improve our knowledge about the aetiology, pathogenesis, prognosis and therapy of MBD.
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  • 20
    Electronic Resource
    Electronic Resource
    Springer
    Child's nervous system 5 (1989), S. 102-106 
    ISSN: 1433-0350
    Keywords: Brain tumors ; Infants ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract In order to compare the validity of CT and MRI, we evaluated results of these studies in 40 children and adolescents suffering from supratentorial and infratentorial midline tumors. Plain and enhanced CT scans were compared with MRI for sensitivity, specificity and capacity to delineate the tumor. These parameters were evaluated by three independent investigators on a scale with four grades of accuracy. The results demonstrate greater sensitivity and better delineation of the tumor with MRI, but greater specificity in diagnosis of tumors with CT studies.
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  • 21
    Electronic Resource
    Electronic Resource
    Springer
    Child's nervous system 5 (1989), S. 201-207 
    ISSN: 1433-0350
    Keywords: Cavernous angioma ; Cerebral angiography ; Computed tomography ; Epilepsy ; MRI ; Surgery
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Cerebral cavernous angioma is a rare vascular malformation at any age and is very rare in childhood. In the literature available to us, we have been able to trace only 50 cases, to which we have added the 6 cases from our own series. The incidence in pediatric group is higher at 0–2 years (26.8%) and at 13–16 years (35.7%). The clinical onset shows epilepsy in 45.4% of cases, hemorrhagic syndrome in 27.3%, intracranial hypertension in 16.4%, and focal neurological deficits in 10.9%. Furthermore, we discuss the neuroradiological features (CT, angiography, and MRI) and the therapy of pediatric cavernous angioma.
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  • 22
    Electronic Resource
    Electronic Resource
    Springer
    European archives of psychiatry and clinical neuroscience 239 (1989), S. 125-126 
    ISSN: 1433-8491
    Keywords: MRI ; Amyotrophic lateral sclerosis ; White matter abnormalities
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Magnetic resonance imaging (MR) of the brain was performed in five patients with amyotrophic lateral sclerosis (ALS) and the findings were evaluated. Two patients had asymmetrical areas of increased signal intensity in the white matter. Such changes are not specific, but some possible explanations for these findings in ALS are considered.
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  • 23
    ISSN: 1573-2630
    Keywords: choroidal nevus ; choroidal melanoma ; MRI ; internal eye wall resection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract A 68-year-old white male had a pigmented choroidal tumor associated with progressive loss of vision. Clinical studies with fluorescein angiography and magnetic resonance imaging suggested a diagnosis of choroidal melanoma. Specimens obtained by internal eye wall resection revealed a choroidal nevus.
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  • 24
    Electronic Resource
    Electronic Resource
    Springer
    European archives of oto-rhino-laryngology and head & neck 246 (1989), S. 262-264 
    ISSN: 1434-4726
    Keywords: Anatomical brain slices ; CT scan ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The authors have used CT scans and MRI to study pathology in anatomical and radiological correlations of brain slices. The CT scan was particularly useful for studying structures at the skull base, although at the level of the posterior fossa such scans could visualize only those tumors that were larger than 8 mm, even after injection. The CT scan was found to be the most useful examination before surgery for facial neuralgia. In contrast MRI gave a precise cisternal course of the trigeminal nerve and its relations with vascular structures.
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  • 25
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 46-47 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Different metal salts have been tried as impregnating reagents for developing TLC separation schemes for some antihistamines on silica gel ‘G’ plates, using a new solvent system benzene + dimethyl formamide + acetic acid (30:10:7). Spots were visualized by spraying with a solution of Dragendroff's reagent.
    Additional Material: 1 Tab.
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  • 26
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
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  • 27
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 10-13 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simplified method for the preparation of wheat germ agglutinin(WGA)-Sepharose 4B by coupling highly purified WGA, prepared by improved affinity chromatography, with BrCN activated Sepharose 4B in a solution of high carbonate buffer is described. The amount of WGA linked to Sepharose 4B was 82.40% (3.07 mg WGA per ml Sepharose 4B). MN blood group antigens of human erythrocyte membranes purified with WGA-Sepharose 4B affinity chromatography showed a single band on sodium dodecyl sulfate/polyacrylamide gel electrophoresis (SDS/PAGE). The yield of the antigens from 400 mL fresh blood was 32-40 mg. The WGA-Sepharose 4B column could be used several times without loss of activity.
    Additional Material: 4 Ill.
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  • 28
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 32-34 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for the unambiguous characterization of DNA photoproducts has been developed. It does not require radio-labelled DNA, or specialized techniques. In the preliminary step, UV-irradiated DNA is hydrolysed to its constituent bases and photoproducts. The photoproducts are then separated from nucleic acid bases using low pressure ion-exchange chromatography on a Dowex 1 × 8 200-400, and an Amberlite CG-50-H+ column. Further separation and purification of photoproducts is carried out on the HPLC Whatman Partisil ODS2 column, using 15% MeOH. The procedure is simple, reproducible and versatile.
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  • 29
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    Biomedical Chromatography 3 (1989), S. 43-45 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Two new solvent systems, n-hexane + propionic acid (26:5, v/v) and chloroform + acetone (29:3, v/v), for the rapid resolution and identification of an 18-component mixture of phenylthiohydantoin amino acids are reported. Using these systems certain difficult combinations of phenylthiohydantoin amino acids are resolved. Two more solvent systems, viz chloroform+acetic acid (27:3, v/v) and chloroform + methanol (30:4, v/v), are developed to resolve phenylthiodantoin derivatives of aspartic and glutamic acids.
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  • 30
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 31
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    Biomedical Chromatography 3 (1989), S. 49-52 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple rapid method for simultaneous ethosuximide and phenobarbital assay in brain tissue, serum and urine has been developed. Extraction of samples from brain tissue and serum were performed with dichloromethane at low pH in the presence of an excess of ammonium sulfate. Glucuronide conjugates in urine samples were hydrolyzed by enzymatic cleavage with β-glucuronidase and then extracted with dichloromethane. The extracts were analyzed using a Spherisorb 5 ODS column and a mixture of acetonitrile, methanol and phosphate buffer (21: 24: 55, v/v) as eluent. No interference was encountered and the method is both precise and reproducible.
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  • 32
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    Biomedical Chromatography 3 (1989), S. 136-138 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high performance liquid chromatographic (HPLC) method for the determination of the anticoccidial and antitheilerial drug halofuginone in bovine plasma was developed. Samples were diluted with acetic acid (10%, v/v) and cleaned up on a Bond Elut C8 column. The analyte was eluted from the extraction column and chromatographed by reversed-phase HPLC using decylamine as a competing-ion reagent. Detection was by UV at 243 nm. Recovery from plasma was 75%, and within-day and between-day coefficients of variation were 5.23 and 6.35% respectively. The specificity and sensitivity of this method (limit of detection in plasma, 1 ng/mL) were sufficiently high to enable us to characterize the time course of the drug in plasma after oral administration of therapeutic doses to cattle.
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  • 33
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 34
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new method based on displacement electrophoresis has been developed for the determination of the total and free concentration of propranolol, a β-adrenergic blocker drug, in plasma. To determine the total concentration the drug is extracted from human plasma into a chloroform + heptane mixture in the presence of ammonia. After evaporation of the solvent mixture the residue is submitted to displacement electrophoresis in a glass tube containing a two-layer polyacrylamide gel. When the propranolol electrophoretically leaves the gel column it is transferred by a buffer flow to the cuvette of a fluorimeter for continuous detection and quantification. The concentration of the free non-protein bound drug can be determined by the same displacement electrophoresis technique following extraction of the plasma sample into the above organic solvent mixture in the absence of ammonia. Alternatively the extraction procedure can be exchanged for dialysis for 1 h. To decrease the risk that large size material might comigrate with propranolol two layers of polyacrylamide are used, one having small pores to retard such material. In addition, we use fluorimetric detection which means that many possible contaminants are not recorded and therefore do not affect a quantitative determination of propranolol.
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  • 35
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    Biomedical Chromatography 3 (1989), S. 255-261 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Analyses of estrogen and progesterone receptors in biopsies of breast carcinoma play a vital role in the selection of patients likely to respond to hormone manipulation. Sucrose density gradient centrifugation has been the reference method in the determination of estrogen receptors in human breast carcinoma cytosols. To reduce assay time and circumvent prolonged manipulation of labile receptor preparations, high performance liquid chromatography techniques in the size-exclusion and ion-exchange modes were compared as potential alternate methods for the rapid separation of receptor isoforms. Multidimensional analyses were performed by reapplying estrogen receptor isoforms obtained from high performance size-exclusion and ion-exchange chromatography to sucrose density gradients and vice versa. This confirmed that the estrogen-binding components identified by high performance liquid chromatography appear to correspond to estrogen receptor species from sucrose density gradients.
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  • 36
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    Biomedical Chromatography 3 (1989), S. 269-271 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive (2 ng/mL) and specific method for the determination of the benzodiazepine antagonist Ro 15-1788 or flumazenil is described. Following a simple extraction, the compound is analyzed by reversed phase high performance liquid chromatography (HPLC) and detection at 245 nm. The method was applied to plasma specimens collected from patients receiving a single dose of this drug.
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  • 37
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and precise method for the quantitation of epomediol in human plasma and urine is described. Each biological sample is added with the internal standard and applied directly to an Extrelut-1 solid-phase column. After absorption the column is eluted with chloroform and the eluate is evaporated to dryness. The residue, reconstituted in ethanol, is analysed by capillary gas chromatography. No interferences from possible metabolites or endogenous constituents can be noted. The method has been applied to human pharmacokinetic studies: the results of a subacute administration to volunteers are presented.
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  • 38
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Malonyl-CoA is a biochemically important compound, formed by an acetyl-coenzyme A carboxylase catalysed reaction. The stability of this short-chain coenzyme A derivative under various experimental conditions is discussed in this article. High-performance liquid chromatography was used for the analysis of the reaction mixture because of its excellent selectivity and sufficient sensitivity. Several variables were investigated as possible stability-influencing factors: pH, magnesium and buffer concentration, reaction temperature and time. The Plackett-Burman screening design was first used for selecting the most important variables, with which a central composite design was constructed. In this way, a response surface was obtained with the percentage remaining malonyl-CoA as a function of magnesium concentration, reaction temperature and time. The usefulness of this approach is demonstrated by obtaining kinetic data from the mathematical function and by the evaluation of the stopping of reaction procedure in the activity assay of acetyl-coenzyme A carboxylase.
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  • 39
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    Biomedical Chromatography 3 (1989), S. 221-225 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Rabbit kidney (RK-13) and human jejunum and ileum (I-407) cells infected with herpes simplex virus type 1, strain F, were radiolabelled with [14C]glucosamine or [35S]methionine for 24 h. The cells were extracted with 1% Triton X-100 and the extracts were separated by gel filtration high performance liquid chromatography. Monoclonal antibody immunoprecipitation of the fractions collected from the column revealed a monomeric glycoprotein D (gD) of 52 - 56 000 molecular weight from RK-13 cells and two monomeric forms of gD, 54 000 and 58 000 molecular weight, from I-407 cells. Densitometry scanning of the autoradiograms from SDS-PAGE showed gD from the RK-13 host cells to be 98.7% pure with the [35S]methionine label and 97.0% pure with the [14C]glucosamine. On the other hand, gD from the I-407 host cells was only 78.6% with the [35S]methionine label and 96% pure with the [14C]glucosamine. This method could provide a means for the isolation of native gD for structural and immunological studies.
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  • 40
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    Biomedical Chromatography 3 (1989), S. 233-240 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The dinitrophenyl (DNP) derivatives of amino acids have found continual application in protein sequencing since Sanger used them for the first time for the sequencing of insulin. Dansyl derivatives of amino acids have been widely used in protein sequencing because of their fluorescent nature. The success of protein sequencing largely depends upon correct identification of such derivatives. The choice for the method of identification is related to cost, the availability of instrumentation and to the sensitivity needed for the analysis. Thin layer chromatography (TLC) is simple and has several advantages over other chromatographic methods. Therefore the literature after 1972 is reviewed for TLC analysis of dansyl- and DNP-amino acids, the two important amino acid derivatives required for identifying protein sequences. Additionally, the literature on the TLC resolution of enantiomeric mixtures of dansyl amino acids is reviewed. Application of various adsorbents, composition of solvent systems and other experimental conditions together with successful resolution data have been discussed. TLC provides a direct and inexpensive method for the resolution of enantiomers, and is fast becoming a sensitive instrumentalized quantitative analytical technique.
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  • 41
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    Biomedical Chromatography 3 (1989), S. 272-273 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An HPLC method for the simultaneous detection of six organophosphorus pesticides (Dimethoate, Ethion, Malathion, Phorate, Phosalone and Parathion) on a Zorbex ODS column using methanol + water (80: 20) as solvent is described.
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  • 42
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A novel analytical method for biological polyamines (putrescine, spermidine and spermine) was developed. Polyamines were separated by ion-pair reversed phase chromatography using a polymer-based octadecyl bonded column. A polyamine oxidase immobilized column worked effectively as a post-column reactor to convert polyamines to hydrogen peroxide which was eventually detected by electrochemical oxidation on platinum electrode. This method required neither tedious derivatization nor gradient elution, permitting us to perform simple and rapid analysis of polyamines. The detection limits were 0.3, 0.6, and 4 pmol injected for putrescine, spermidine, and spermine, respectively with a linear range of two to three orders of magnitude. Chromatograms obtained with samples from human urine and rat brain homogenates demonstrated the high sensitivity and selectivity of the method.
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  • 43
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    Biomedical Chromatography 3 (1989), S. 276-278 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Highly purified monomeric human plasma lecithin:cholesterol acyltransferase (LCAT), completely free of apolipoprotein D, has been chromatographed on a MonoQ HR 5/5 anion exchanger. LCAT eluted as symmetrical peaks after 12.8 min and 14.8 min at pH 5.0 and pH 6.0, respectively, using a linear NaCl gradient. The corresponding concentrations of NaCI effecting desorption of LCAT from the anion exchanger were 125 mM and 175 mM. At both pH values human serum albumin eluted earlier and was well separated from the enzyme. Rechromatography of LCAT in the eluates from these experiments at acid pH, on high performance gel filtration, demonstrated absence of aggregation. The nonspecific adsorption during anion exchange chromatography at pH 5.0 and pH 6.0 was negligible, as demonstrated by a linear relationship between injected amounts of LCAT and recorded peak areas for a 2-20 μg protein range. Zone immunoelectrophoresis assay indicated unaltered immunoreactivity of the eluted LCAT.
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  • 44
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The chromatographic behaviour of the membrane-attached variant surface glycoprotein (mfVSG) of bloodstream forms of Trypanosoma brucei brucei AnTat 1.1 A preparations were studied by reversed phase high performance liquid chromatography (RP-HPLC). Among the different preparation procedures used, only the trifluoroacetic acid extraction gave a mfVSG preparation which was eluted from the RP-HPLC column. As well as for the soluble variant surface glycoprotein (sVSG) it was found that different mfVSG forms were eluted at different organic solvent concentrations from the RP-HPLC column. In addition, in preliminary studies, we have attempted to characterize the factors responsible for the trypanosome surface coat assembly. Using chromatographic techniques (RP-HPLC and thin layer chromatography), the results suggest a close relationship between the content of lipid-containing species and the heterogeneity of mfVSG preparation.
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  • 45
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 46
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. ii 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 47
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. iii 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 48
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    Biomedical Chromatography 3 (1989), S. 153-156 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An automated column-switching HPLC system is described for the simultaneous determination of midodrine, an alpha-adrenergic stimulating drug, and its active metabolite, ST-1059. Serum or plasma (850 μ L) is directly injected onto a RP 18 (30 μm particle size) pre-column (9 × 4 mm ID) which acts as an on-line liquid-solid extractor and analyte enrichment system. The injection is followed by washing steps. The fraction containing the analytes is transferred onto an analytical RP18 column via step gradient elution where the final analysis is performed. Fluorescence detection is used (λex 290 nm and λem 322 nm), and method detection limits of 0.8 ng/mL plasma were reached. These were sufficiently low to determine the plasma concentration-time profiles for both compounds following oral administration of 2.5 mg and 5 mg midodrine hydrochloride. The assay in serum or plasma was linear in the range of 1 to 15 ng analyte/mL, the recovery was 〉95%, and the reproducibility was sufficient. The assay was rugged and was maintained by routinely changing the home-made, dry packed pre-column every 20th serum injection.
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  • 49
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    Biomedical Chromatography 3 (1989), S. 177-179 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method has been developed for the separation and measurement of fluvoxamine in human plasma by high performance liquid chromatography. The method uses metapramine as an internal standard and provides a limit of detection of about 1.5 ng/mL for fluvoxamine. At a concentration of 25 ng/mL, fluvoxamine could be measured within a coefficient of variation of ±5.82 of the mean and at 100 ng/mL within a CV of ±2.78 of the mean. The method has been applied to the analysis of plasma from patients undergoing fluvoxamine therapy.
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  • 50
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Conditions for unblocking reversible chemical modifications such as maleylation or citraconylation ‘in situ’ at the N-terminus of proteins after transfer of proteins to immobilon membranes from SDS-PAGE are described. Demaleylation or decitraconylation occurred at 55°C in 70% formic acid (pH 1.50) during 60 min. During the unblocking reaction, Coomassie blue dye was completely removed, resulting in superior high performance liquid chromatographic separation of phenylthiohydantoin-amino acid (PTH-AA) after Edman degradation (automatic gas phase sequencer). The protein fixed on the matrix after demaleylation and removal of Coomassie blue was not degraded. The possible cleavage at the aspartyl-prolyl peptide bonds was considered, but no side reaction was observed. Furthermore, the incubation time in 70% formic acid at 55°C could be reduced to 10 min in the absence of maleylation of the starting material, and this was suitable for the removal of Coomassie blue and the quantification of phenylthiolhydantoin-amino acids (PTH-AAs) by HPLC. The yield from the starting protein through SDS-PAGE, blotting, and Edman degradation to quantitative analysis of PTH-aminoacid(s) by HLPC was established.
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  • 51
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 52
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 53
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    Biomedical Chromatography 3 (1989), S. 192-195 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An HPLC method with direct sample injections and column switching was investigated for the analysis of drugs in tissue homogenates. The appropriate precolumn packings and analytical column packings were surveyed in order to obtain quantitative recovery. The use of a large bore end-fitting filter for the precolumn avoided the interference due to minute tissue particles. A minicolumn was used to trap the analyte or clean up the sample. The method was applicable to hydrophilic as well as hydrophobic drugs in liver, kidney or heart tissues, and has been extensively used in the determination of drugs in centrifugal cell fractions such as the nucleus, mitochondria and microsome.
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  • 54
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    Biomedical Chromatography 3 (1989), S. 196-198 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A quantitative method for the determination of estriol (E3) and creatinine (C) in random urine by high performance liquid chromatography is described. The mobile phase was a mixed solution of methanol and phosphate buffer (0.025 M, pH 6.5) and the detection wavelength was at 205 nm. The method was simple, rapid and accurate. The OCV for E3 and C using this method were 1.7 - 3.4% and 2.2 - 2.5%, respectively. The RCV for E3 and C were 6.2 - 7.0% and 4.5 - 6.9%, respectively. The recoveries were 87 - 104% for E3 and 98 - 103% for C, respectively. The method has been used for clinical determinations.
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  • 55
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Different strategies for HPLC separation, including molecular sieving, ion-exchange, and hydrophobic interaction as well as reversed phase chromatography, were used to study molecular components in human cerebrospinal fluid (CSF). The separations were followed by photodiode-array UV detection, which is a recently developed technique allowing a direct and rapid discrimination between peptides and proteins differing in their content of aromatic amino acids. By the various HPLC techniques in conjunction with diode-array detection it was possible to identify and characterize several protein and peptide components present in CSF. The procedure also allowed quantitative analysis of CSF proteins using minute amounts of the fluid.
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  • 56
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A newly developed method for the simultaneous extraction and quantitation of the unconjugated levels of the catecholamine metabolites vanilmandelic acid (VMA), 3-methoxy-4-hydroxyphenylethylene glycol (MHPG) and homovanillic acid (HVA) in plasma by high performance liquid chromatography with electrochemical detection was modified and applied to studies of human saliva. The assay had a mean coefficient of variation under 3% for each of the metabolites. Levels of plasma VMA, MHPG and HVA were measured in 28 normal subjects and compared to their saliva levels, obtained before and after stimulation by mastication. Significant correlations were found between plasma and saliva MHPG and HVA, but there was no correlation between plasma and saliva VMA. Salivary MHPG and HVA can be reproducibly assayed and may be useful tools for indications of changes in central and peripheral catecholamine metabolism.
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  • 57
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    Biomedical Chromatography 3 (1989), S. 5-9 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive liquid chromatography method has been developed using electrochemistry for the determination of leukotrienes in biological fluids. Biological specimens are treated with 3,5-dinitrobenzoyl chloride in acetonitrile which undergoes rapid reaction with hydroxyl groups of non-peptidic leukotrienes in the presence of pyridine and with amino groups of peptidic leukotrienes in the presence of potassium tetraborate buffer. The resulting dinitroben-zoate derivatives of leukotrienes are highly electroactive, suitable for reduction or oxidation at moderate potentials by an electrochemical detector. In reductive mode at -0.7 V or oxidative mode at + 1.15 V potentials, the lower limits of detection for leukotriene derivatives were approximately 8±3 pg and 70 ± 16 pg respectively, with a signal-to-noise ratio of 5 to 1. This method was applied to the detection of leukotrienes in plasma, nasal and bronchial fluids of patients with asthma.
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  • 58
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new capillary GC method is described for the compositional analysis of the three main gangliosides isolated from adult human myometrium. The sample was subjected to methanolysis, acetylation and trimethylsilylation which allows all the constituents to be analyzed simultaneously. The predominant ganglioside was found to be GD3, with GM3 and GT1b the next most abundant.
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  • 59
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A gas chromatographic-mass spectrometric (GC/MS) method for analysis of Δ1-tetrahydrocannabinol (Δ1-THC) in human fat samples is described. The fat sample, obtained from heavy marihuana users 1 week before and 4 weeks after smoking, is homogenized in hexane + 2-propanol, centrifuged, and the supernatant mixed with Lipidex 5000. The solvent is evaporated and the dried gel is packed in a glass column. Δ1 -THC is eluted from the column with methanol + water + acetic acid, diluted with water and the eluent is passed through a bed of Octadecylsilanebonded silica. After washing and drying, the retained Δ1-THC is eluted with hexane, derivatized with N-methyl-N-(t-butyl-dimethysilyl)trifluoroacetamide (MTBSTFA) and finally purified by HPLC on an Octadecyl SI 100 column in methanol. The amount of Δ1-THC is determined by GC/MS, using selected ion monitoring, and a deuterated internal standard. The recovery of Δ1-THC is about 80%, and the concentration of Δ1-THC in the fat samples analysed ranged between 0.4 and 193 ng/g wet tissue.
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  • 60
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The peroxyoxalate chemiluminescence detection of biological thiols combined with high-performance liquid chromatography (HPLC) is described. SH groups of the thiol compounds including glutathione (GSH), cysteine, N-acetylcysteine, cysteamine, and D-penicillamine were labelled with N-[4-(6-dimethylamino-2-benzofuranyl)phenyl]maleimide (DBPM), a specific fluorogenic reagent for SH group. The labelling reaction was carried out at 60°C for 30 min and at pH 8.5 and a sample of the resulting reaction mixture was subjected to HPLC. Five kinds of labelled thiols were separated within 12 min on ODS-80 column (150 × 4.6mm ID; 5 μm) and detected in the ranges from 500 fmol to 2 pmol/100 μL (cysteamine and N-acetylcysteine), to 3 pmol/100 μL (cysteine) and to 5 pmol/100 μL (GSH and D-penicillamine). The lower detection limits were from 7 fmol (cysteamine) to 113 fmol (GSH) per 100 μL (S/N = 2). The method was applied to the determination of thiols in a rat liver. The amounts of glutathione and cysteine were 1.23±0.15 μmol/g (n = 5) and 0.15±0.04 μmol/g (n = 5), respectively.
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  • 61
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    Biomedical Chromatography 3 (1989) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 62
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid assay employing HPLC with electrochemical detection for catechol-O-methyltransferase (COMT) activity in red blood cells is described. Enzyme activity is determined from erythrocyte lysates using S-adenosyl-L-methionine as methyl donor and 3,4-dihydroxybenzoic acid as substrate. The 3-O- and 4-O-methylated reaction products are measured by high-performance liquid chromatography with electrochemical detection. Human erythrocyte soluble form of COMT had Km values of 6.1 μM and 26.0 μM for S-adenosyl-L-methionine and dihydroxybenzoic acid, respectively. The mean O-methylation ratio for the soluble form of COMT was 5.3. An O-methylation ratio of 15.5 was estimated in the membrane fraction of an erythrocyte pool from three samples. The activities of soluble COMT in erythrocytes of some animal species are also reported. The procedure is easily automated, and a large number of samples can be processed during one working day.
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  • 63
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    Biomedical Chromatography 3 (1989), S. 72-74 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A reversed-phase HPLC system with 88% methanol in 1 M ammonium acetate buffer pH 5.35 as the mobile phase on an ODS column was used to analyse pheophorbides a, a', b, b' and pyropheophorbides a and b. Pyropheophorbides a and b were found in samples obtained from silkworm excrement but not from spinach leaves though the preparation methods used were the same. This difference suggests that chlorophylls undergo metabolism in the body of silkworm to give pyrochlorophyll derivatives.
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  • 64
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    Biomedical Chromatography 3 (1989), S. 82-87 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Hormone-sensitive lipase (HSL), the enzyme controlling the rate of adipose tissue lipolysis and also possibly involved in the regulation of steroidogenesis, has been purified from bovine omental adipose tissue. Partially detergent-solubilized, delipidated and purified HSL was obtained through step-elution at conventional DEAE ion-exchange chromatography, followed by concentration on hydroxylapatite. High performance hydrophobic interaction chromatography (HPHIC) on phenylsilica then resulted in an increase of HSL protein purity from 2% to more than 70%. Final purification of the enzyme to apparent homogeneity (〉95% protein purity), concentration and removal of most of the detergent was obtained by high performance cation exchange chromatography on Mono S. At least 0.5 mg of highly stable HSL was obtained from 5 kg of bovine omental fat within four working days. The purified lipase had a lower specific activity than previously reported for the corresponding rat enzyme but the preparations have proved very useful for enzyme structure studies and as an antigen.
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  • 65
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    Biomedical Chromatography 3 (1989), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 66
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    Biomedical Chromatography 3 (1989), S. 95-104 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 3 Ill.
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  • 67
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Fluorescein isothiocyanate (FITC)-labelled asialotransferrin and pyridyl aminated oligosaccharides were prepared from asialotransferrin and human milk using affinity chromatography and high performance liquid chromatography (HPLC), respectively. These substances were incubated with galactosidase or sialyltransferase and then examined by lectin affinity HPLC. The elution patterns changed according to the period of incubation and amount of enzyme. This analytical method using lectin affinity HPLC with fluorescence labelled glycoprotein or oligosaccharides as the substrates has great value for detecting these enzyme under the same chromatographic conditions. In addition, differences were noted in the activity of β-galactosidase toward oligosaccharides having the Gal β(1 → 3)GlcNAc or Gal β(1 → 4)GlcNAc structure at reducing termini.
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  • 68
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The isolation and properties of lactoferrin from human breast milk and from neutrophilic granulocytes were investigated. Human breast milk lactoferrin was purified by means of heparin-sepharose or Cibacron Blue affinity chromatography. Quantitative recovery using these two methods was comparable but Cibacron Blue affinity chromatography allowed for isolation of a more homogenous protein. Lactoferrin could only be isolated from human neutrophilic granulocytes by sequential use of antibody affinity followed by non-specific affinity chromatography. Both breast milk lactoferrin and granulocyte lactoferrin were separated into apo and iron-rich species by SDS polyacrylamide gel chromatography. Iron binding is accompanied by a conformational change in tertiary structure associated with more rapid electrophoretic migration. The isoelectric point of both human breast milk lactoferrin and human granulocyte lactoferrin is 5.5 - 6.2. Both types of lactoferrin have similar iron binding properties with release of iron from the one binding site occurring at pH 5.2 - 6.0 while the other binding site holds on to iron down to pH 3.6 - 3.2. Despite the high affinity for iron the percentage saturation of native lactoferrin is low, that for breast milk lactoferrin averaging 12 - 25% and that for granulocyte lactoferrin 〈 10%.
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  • 69
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Human trypsin inhibitor (home prepared), lactalbumin, trypsinogen, carbonic anhydrase, and bovine serum albumin were submitted to succinylation and their molecular masses were determined by SDS-PAGE according to the method of Weber and Osborn (1969 J. Biol. Chem. 244, 4406) before and after chemical modification. High estimates of their molecular masses were obtained. The monomer and dimer of arrowhead inhibitor proteinase-B (Chinese vegetable legume) obtained after chemical crosslink(s) were also submitted to SDS-PAGE and their apparent molecular masses were also determined and compared to the native arrowhead inhibitor proteinase-B. Abnormally high estimates of their molecular masses were obtained. Our results agree with those in the literature.
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  • 70
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    Biomedical Chromatography 3 (1989) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 71
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    Biomedical Chromatography 3 (1989), S. 114-117 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A HPLC method for the quantitative determination of 5-hydroxy-3-indoleacetic acid (5-HIAA) in urine is described. The method is based on ion-pair chromatography, reversed phase (RP) column material and specific fluorimetric detection at 300 nm and 355 nm. Sample preparation and gradient elution were avoided by using a column-switching technique. The sensitivity of the assay was excellent for clinical routine analysis, with a detection limit of 0.2 mg/L 5-HIAA. No endogenous or exogenous interference problems arose. Intra- and interassay precision was good, with observed coefficients of variation of 1.5 to 2.6% and 2.1%, respectively. Recoveries were 93 to 98%. The system described can be used for clinical diagnosis and therapy follow-up of carcinoid tumors. It has been running for over a year without disturbances and with a minimum of technical attendance.
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  • 72
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    Biomedical Chromatography 3 (1989), S. 127-130 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The soluble form of catechol-O-methyltransferase (EC 2.1.1.6.) from rat liver was purified to homogeneity by high-performance anion-exchange chromatography and high-performance gel-filtration chromatography. The specific activity of the final pool was 270 U/mg protein. The purification was 1180-fold and recovery of the enzyme activity was 15%. During this rapid and gentle purification there were no problems with loss of activity, and the estimated half life of the final purified enzyme pool was 5.5 days at +4°C. The only additive used was phenylmethylsulfonylfluoride in the homogenizing buffer.
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  • 73
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Analytical conditions of prepurification extraction and HPLC separation were optimized for determination of urinary serotonin and tryptamine. Under optimal conditions, serotonin, tryptamine and an internal standard were extracted with 15% v/v n-propanol in diethyl ether from urine samples alkalized with a phosphate buffer (0.75 mol/L, pH 10.0), and then they were re-extracted into an HCI solution (0.1 mol/L). Purified indoleamines were simultaneously separated by reversed-phase ion-pair HPLC with native fluorescence detection. Urinary serotonin and tryptamine were selectively determined within about 45 min per sample for the whole procedure. Analytical recovery, reproducibility and detection sensitivity were satisfactory for pursuing time-dependent changes in indoleamine levels. Urinary excretion profiles of serotonin and tryptamine in subjects dosed with L-tryptophan were successfully analyzed by our method.
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  • 74
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    Biomedical Chromatography 3 (1989) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 75
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    Biomedical Chromatography 3 (1989), S. 241-245 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A practical procedure for isolating and purifying glycopeptides is described, viz. enzymatic hydrolysis - gel permeation chromatography - ion exchange chromatography - reversed phase HPLC. Using this procedure 28 glycopeptides from hen ovalbumin have been isolated some of which hitherto have not been identified. Water was a suitable mobile phase for preparing pure glycopeptides, and control of column temperature was important for good separations and reproducible retention times. Structural confirmation was by fast atom bombardment mass spectrometry.
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  • 76
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method is described to isolate rapidly human hemoglobin-benzo[a]pyrene diol epoxide adducts. A combination of 300 Å pore size C4 reversed phase HPLC to effect separation of adducted protein from native protein, and μ-bore C18 reversed phase HPLC to isolate and partially characterize proteolytic peptide adducts (by UV), was used.
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  • 77
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple, accurate and precise procedure for the quantitation of itazigrel (a potent lipophilic inhibitor of collagen and arachidonic acid-induced aggregation being studied for its effects on peripheral vascular disease) from granulated rodent diet is presented. The drug was extracted from rodent diet using methanol + water (80:20) following dissolution of the diet in water. Samples of the supernatant were injected into the HPLC and the eluent was monitored with a fluorescent detector (λex = 320 and λem = 430) to achieve analytical specificity. Interday coefficients of variation of the calibration curve slope were ±6% on standards between 0 and 1000 μg/g. Potency and homogeneity of the drug spiked diet prepared over a 1 year interval at 70,200 and 600 μg/g was 99.3 ± 2.5%, 100 ± 1.8%, and 101 ± 1.9% of label, respectively. Samples prepared for chromatography were stable for 24 h at 20°C, and drug in diet was stable for 102 days when protected from light and stored at 20°C.
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  • 78
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    Biomedical Chromatography 3 (1989), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 79
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    Biomedical Chromatography 3 (1989), S. 183-185 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The release and content of the excitatory amino acid neurotransmitters glutamate and aspartate in rat striatum were determined by liquid chromatography/electrochemistry. This determination was based on precolumn off-line derivatization of the amino acids with o-phthaldialdehyde and 2-mercaptoethanol (OPT/2-MCE), and the adducts formed were separated under isocratic conditions and oxidized on a glassy carbon electrode at moderate potential (+0.6 V). The standard and the extracted glutamate when derivatized with OPT/2-MCE produced similar electrochemical and chromatographic characteristics. The detection limit of glutamate was 0.5 pmol. Depolarization induced by the high potassium medium (40 mmol/L) enhanced the release of glutamate and aspartate from superfused rat striatum, whereas the efflux of glutamine remained unchanged. Perfusion (for 60 - 70 min) removed 50 - 80% of the free amino acid content of striatal tissue. The method described here is useful in neurochemical investigations of the brain amino acid neurotransmitters.
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  • 80
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    Biomedical Chromatography 3 (1989), S. 209-212 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for the determination of cyanide in human urine has been developed. The method is based on the reaction of cyanide with 2,3-naphthalenedialdehyde and taurine to give a fluorescent product for reversed-phase HPLC separation and fluorometric detection. After centrifugation followed by dilution of urine samples, the specimens could be analysed directly by this method. The recovery of cyanide added to urine at concentration levels of 50 - 1000 pmol/mL was 85 - 96%. The detection limit of cyanide was 30 pmol/mL in urine. The method was successfully applied to the analysis of urine from smokers and nonsmokers. The mean concentrations of cyanide were found to be 215 pmol/mL for the former and 84 pmol/mL for the latter.
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  • 81
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    Biomedical Chromatography 3 (1989), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 82
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    Biomedical Chromatography 3 (1989), S. 226-232 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple, selective and very sensitive assay is described for the quantification of physostigmine in blood, plasma and urine. The most appropriate solid phase column was selected after a systematic investigation of nine types of phase. The conditions for solid phase extraction were optimized using [3H]physostigmine so that the overall recoveries were 〉90%. Physostigmine was retained on alkaline treated cyanopropyl columns and eluted into the minimum volume of methanol, obviating the need for an evaporation step. Extracted samples were quantified by HPLC with a three electrode coulometric detection system. The limit of detection was 50 pg/mL for a 0.5 mL plasma sample. The precision (CV) for 0.5 mL plasma samples containing 50 pg was 8.1%. Application of the method to plasma, blood and urine samples is presented.
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  • 83
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    Biomedical Chromatography 3 (1989), S. 251-254 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Meibomian secretions from the hamster were hydrolysed with base and examined as TMS, [2H9]TMS, methyl ester/TMS, picolinyl ester/TMS and nicotinate/TMS derivatives by capillary GC/MS. Over 90 compounds, representing over 89% of the hydrolysed fraction, were identified. Fatty acids with chain lengths from 10 to 32 carbon atoms were found, the most common of these were in the C15 to C18 and in the C25 to C30 regions. Chain types were predominantly iso or anteiso branched, mono-unsaturated (C16 and C18) and straight. Fatty alcohols were mainly from the iso or anteiso series and tended to have longer chain lengths; the major alcohols had anteiso-25 and 27 and iso-26-chains. In these respects the secretions were similar to those reported earlier from other species, although fewer mono-unsaturated compounds with longer chains (C20 to C30 region) were found than in the rat and human. The steroid fraction was characterized by a larger number of compounds than normally present in secretions of this type. The major compound was cholesterol, in common with that in all other examined species except the rabbit.
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  • 84
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and precise method was developed for the separation of nucleosides including modified nucleosides and oligonucleotides. Nineteen kinds of nucleosides were completely separated by HPLC using an ODS column (TSK-gel ODS 80TM) and aqueous mobile phases. The RNA molecule was digested by base restrictive RNase (RNase A, RNase T1) and the digests were separated chromatographically into each oligonucleotide. The nucleoside composition of an oligonucleotide was then determined by this analytical system. It is thus possible to fit the oligonucleotide in the original RNA molecule by using modified bases as markers. The reaction site of quinacrine mustard for tRNAPhe (from yeast) could be determined by this analytical system.
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  • 85
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    Biomedical Chromatography 3 (1989), S. 262-265 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high performance liquid chromatographic method is described for the simultaneous determination of furosemide and bumetanide in horse plasma. The C8 (3 μm) reversed phase column (4.8 × 150 mm) provided clear separation of furosemide and bumetanide with other components present in the horse plasma. The detection limit for both the drugs was 10 ng/mL. Both drugs were stable in plasma (at natural or acidic pH) for up to 24 h. The method is sufficiently sensitive to detect furosemide levels in plasma obtained from horses receiving a therapeutic dose of furosemide.
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  • 86
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    Journal of Chemometrics 3 (1989), S. 601-608 
    ISSN: 0886-9383
    Keywords: Gas phase flow injection analysis ; Membrane-differentiated analysis ; Multicomponent determinations ; Successive linear regression ; Successive regression in fiduciary region ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A membrane-discriminated gas phase analyzer is proposed for multicomponent determinations. Nitrogen gas flows countercurrent through outer and inner channels in a tube-in-tube arrangement. The only communication between the two channels occurs through a 500 μm aperture covered by a porous PTFE membrane. A mixture of organic compounds (up to four components) is injected into the inner channel by a heated backflushed injector and the sample components diffusing into the outer channel are monitored by a flame ionization detector (FID). A calibration set, consisting of pure components, binary, ternary and quaternary mixtures (a total of 64 samples), provides the known data base: temporal profiles of the FID output as a function of sample composition. Although the overall response behavior is not a linearly additive function of individual analyte concentrations, the use of successive inverse multiple linear regression (while continually altering the choice of the calibration samples considered for the forward regression, on the basis of the most recent values of the predicted unknown sample composition) is shown to yield analytical results for unknown samples that are in good agreement with their true values.
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  • 87
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    Journal of Chemometrics 3 (1989), S. 609-609 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 88
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    Biological Mass Spectrometry 18 (1989), S. 174-176 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Plasma levels and urinary excretion of mevalonate were reported to be correlated with cholesterol biosynthesis. Evaluation of mevalonate concentration in plasma and urine represents therefore a non-invasive method for studying the modifications of cholesterol synthesis. A method is described here by wich mevalonate in plasma and urine is determined by the selected ion monitoring technique after extraction as mevalonolactone and conversion into the trimethylsilyl ether. Linear responses were obtained in the evaluation of mevalonate added to plasma in the 10-100 ng/ml (r 〉 0.995) and to urine in the 50-1000 ng/ml concentration ranges, respectively. Identity of mevalonate in plasma and urine was confirmed by high-resolution mass spectrometry.
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  • 89
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) mass spectrometry was used to characterize the pyochelin complexes of iron and zinc. Ferripyochelin readily forms the [M + H]+ and [2M + H]+ ions in a glycerol matrix. The molecular ion was 2.5 fold more abundant when acetic acid was present. Iron was shown to be present in the iron-pyochelin complex as the ferric ion by wet chemical methods. Differentiation between ferric and ferrous ions by FAB was not successful owing to the FAB reducing environment. Ferric ions were reduced by FAB to ferrous ions in the following model salts - ferric chloride, ferric nitrate and ferric sulfate - when dissolved in either glycerol, thioglycerol or the magic bullet matrix. Ferric and ferrous chloride salts gave virtually identical spectra with a glycerol/acetic acid matrix. Zinc-pyochelin readily forms the [M + H]+ and [2M + H]+ ions, but only when acetic acid was present in the glycerol matrix. The FAB mass spectrum of zinc-pyochelin exhibited various fragmentations which can be used in structural analysis. Linked-scan at constant B/E and accurate mass data were used to characterize the fragmentations of the zinc-pyochelin complex. Metastable analysis allowed the fragmentation pathway of zinc-pyochelin to be determined.
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  • 90
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    Biological Mass Spectrometry 18 (1989), S. 207-217 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact (EI) mass spectra of 2,6-di-tert-butyl-4-methylphenol (BHT) and certain of its alteration products are described in detail. Accurate mass measurements confirm the elemental compositions of important fragment ions in the EI spectra. Collisionally activated mass spectra are also used to study fragmentation and suggest common ion structures. The reference spectra provide the basis for identifying various alteration products of BHT by capillary gas chromatography/mass spectrometry (GC/MS) without the necessity of isolating individual components. Application of GC/MS is made to three studies: (i) pyrolysis of hydroperoxy-BHT as a potential pathway to alteration products in food; (ii) GC/MS pyrolysis of hydroperoxy-BHT as a model study; and (iii) alteration of BHT in ethanol/water as a food-simulating solvent.
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  • 91
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    Biological Mass Spectrometry 18 (1989), S. 363-372 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The MI and CA spectra of selected positive and negative ions generated by fast atom bombardment (FAB) of the stereoisomeric aldohexoses can be used to differentiate among these isomers, without prior derivatization or addition of other substances. The main fragmentation routes were traced and compared to those of some 2- and 6-deoxyaldohexoses, which appeared to be suitable model compounds. In both positive and negative ion FAB mass spectrometry, the OH group at the C-2 position plays an important role in the fragmentation reactions of the pseudomolecular [M + glycerol + H]+ and [M - H]- ions.
    Additional Material: 1 Ill.
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  • 92
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 387-393 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chicken intestinal calbindin-D28k is an intracellular protein which is believed to have a fundamental role in vitamin D-mediated transport of calcium. A mapping approach based on 252Cf plasma desorption mass spectrometry (PD mapping) was used to screen the DNA-deduced sequence of calbindin-D28k for sequence changes and posttranslational modifications. In the PD mapping experiment, purified calbindin-D28k was cleaved with cyanogen bromide and the resulting peptides were subjected to PD mass spectrometric analysis either as a mixture or as high-performance liquid chromatography isolated fractions. The DNA-derived primary structure of calbindin-D28k was confirmed by rapid PD mass spectral identification of the CNBr peptide fragments, and the nature of the N-terminal blocking group was readily determined to be an acetyl group. The relatively non-destructive nature of the PD mass spectrometric analysis allowed the mapping of the N-terminal peptide through an additional in situ V8 protease enzymatic reaction.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 93
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A current limitation in the use of fast atom bombardment (FAB) mass spectrometric mapping of peptide mixtures, derived from enzymic digestion of proteins, is that most of the hydrophilic peptides are not observed. However, it has been demonstrated from previous work that esterification of the peptide mixture results in the detection of almost all peptides in FAB mass spectrometry. This strategy of FAB mapping was applied to the protein actinidin, isolated from an Italian variety of Actinidia chinensis. Two of the 12 tryptic peptides in FAB mass spectrometry did not exhibit molecular ions predicted from the known sequence of actinidin isolated from the New Zealand variety of A. chinensis. The two peptides were isolated by high-performance liquid chromatography, subjected to Staphylococcus aureus V8 protease digestion and sequenced by gas-phase microsequencing. Nine changes in amino acid composition were detected using the rapid and powerful combination of FAB mass spectrometric mapping and gas-phase microsequencing.
    Additional Material: 1 Ill.
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  • 94
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metabolism of 17α-methyl-17β-hydroxy-2-oxa-5α-androstan-3-one (oxandrolone) in man has been investigated by gas chromatography/mass spectrometry. After oral administration of a 10 mg dose to man, five metabolites were detected in the free fraction of the urinary samples. Oxandrolone, the major compound excreted in urine, was detected within 72 h after administration. During this period 35.8 and 8.4% of the administered dose was excreted as unchanged oxandrolone and 17-epioxandrolone, respectively. In addition, minute amounts of 16α- and 16β- hydroxyoxandrolone and a δ-hydroxy acid resulting from the hydrolysis of the lactone group of oxandrolone were detected in the urine samples 8-60 h after administration. Furthermore, the susceptibility of oxandrolone to hydrolysis was investigated under several pH conditions. Extraction and fractionation of steroidal metabolites was achieved by using C18 and silica Sep Pak™ chromatography. The mass spectra of the metabolites are presented and major fragmentation pathways discussed.
    Additional Material: 10 Ill.
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  • 95
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An increasing amount of evidence is accumulating to support the proposal that steroidogenesis can occur by a sesterterpene pathway as well as the cholesterol pathway. Key intermediates on the sesterterpene pathway are 23,24-dinor-5-cholen-3β-ol (guneribol) and some of its metabolites, e.g. 23,24-dinor-4-cholen-3-one (guneribone). It has been reported that these intermediates are biosynthesized and converted to steroid hormones by a range of endocrine tissues in vitro. Monitoring the pentafluorobenzyloxime derivatives by negative ion chemical ionization mass spectrometry in the electron capture mode provided evidence for the presence of guneribone in extracts of bovine testicular and human adrenal tumour tissue. Complementary evidence was obtained from gas chromatographic/tandem mass spectrometric data generated on a triple-quadrupole instrument by monitoring daughter ions (in the multiple ion detection, MID mode) of the molecular anion of derivatized guneribone in both standards and tissue extracts. The present findings that sesterterpene pathway intermediates are present as endogenous compounds in tissue extracts, together with the previously reported radiochemical data, give further support to the sesterterpene pathway hypothesis.
    Additional Material: 5 Ill.
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  • 96
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic/mass spectrometric analytical procedure is described to determine glycols in plasma as cyclic butyl boronate esters. The method, involving a pre-deproteinization step, required only 0.25 ml of plasma and a short time (20 min) to react with the derivatizing agent (butyl boronic acid). The gas chromatographic separation on a CP Sil 8 CB silica capillary column coupled to a mass detector assured a complete identification of the compounds. The analytical recoveries (〉95%) with low coefficient of variation (4-11%) assured the feasibility of the method over a concentration range from 5 to 1000 μg ml-1 for each glycol. The lower detection limits, namely 1-5 μg ml-1, confirmed the sensitivity of the method.
    Additional Material: 3 Ill.
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  • 97
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 603-612 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of tetradeuterated 10-methylundecanoic acid, dideuterated tetracos-2-enoic acid, (1-14C)pristanic acid and (1-14C)tetracos-2-enoic acid using the Favorsky rearrangement are described. They will be used for studies of long-chain fatty acid metabolism in patients. The positions of isotope labelling were determined by mass spectrometry.
    Additional Material: 12 Ill.
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  • 98
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 617-619 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Negative ion fast atom bombardment mass spectrometry is used to verify the sequence of oligodeoxyribonucleotides containing a single modified nucleotide. Both the position in the sequence and the molecular weight of the modified nucleotide can be determined from the 3′ and 5′-phosphate sequence ions which are prominent in the mass spectrum.
    Additional Material: 2 Ill.
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  • 99
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 620-623 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A number of sulphonyl hydrazones and derivatives have been synthesized and tested for biological activity as pesticides during the crop protection research programme at the Hatfield Polytechnic. A recent comparative ionization study of some of these compounds using electron impact (EI), fast atom bombardment (FAB) and various chemical ionization methods showed FAB mass spectrometry to be the optimum technique to use in terms of molecular weight information obtained. This study compares the FAB mass spectral data in positive and negative ion mode using an alternating positive and negative ion detection system.
    Additional Material: 4 Ill.
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  • 100
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermospray liquid chromatography/mass spectrometry (LC/MS) interface has had a major impact on the direct analysis of the metabolic fate of xenobiotics in complex biological media. This paper outlines the rapidity and power of the LC/MS approach, and shows how detailed structural information can be obtained without recourse to individual compound isolation. This provides a great saving in time and effort. The additional specificity of liquid chromatography/tandem mass spectrometry is highlighted in identifying the sites of metabolic transformation. The ability to handle biological samples with little or no clean-up using wide high-performance liquid chromatographic gradients is a key feature of the success of this methodology.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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