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  • 1990-1994  (1,556)
  • 1992  (1,556)
  • Analytical Chemistry and Spectroscopy  (1,522)
  • English poetry., lcsh
  • MRI
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Years
  • 1990-1994  (1,556)
Year
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Neurosurgical review 15 (1992), S. 125-133 
    ISSN: 1437-2320
    Keywords: Angiography ; cavernous angioma ; CT ; epilepsy ; hemorrhage ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract We report 14 cases of intracranial cavernous angioma, analyzing the clinical features, with special reference to the risk of bleeding, radiological images and treatment in these and in 153 published cases, 167 in all. Cerebral hemorrhage occurred in 44%: typical (intraparenchymal or subarachnoid) in 24.6%, and masked by epilepsy, headache or neurological deficits in 19.2%. In patients with the typical hemorrhagic pattern posthemorrhagic mortality was 12.2%. Of the patients who had a hemorrhage 42.5% were left with more or less disabling neurological deficits, and 16.4% had a rebleed. In discussing treatment we consider four groups of intracranial cavernous angioma: A) symptomatic in a zone of low surgical risk; B) asymptomatic with low surgical risk; C) symptomatic with high surgical risk; D) asymptomatic with high surgical risk. The treatment is surgical, except in the high risk asymptomatic variety, best followed initially with sequential CT scan and MRI and then considered for surgery if the lesion becomes symptomatic, increases in size or presents neuroradiological signs of bleeding.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    The international journal of cardiovascular imaging 8 (1992), S. 249-254 
    ISSN: 1573-0743
    Keywords: Marfan ; MRI ; aortic dilatation ; dissection ; symptomatic ; asymptomatic
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Marfan's syndrome is a connective tissue disorder, which mainly affects the cardiovascular system, together with ocular, skeletal and connective tissue. The cardiovascular manifestations in particular determine the mortality of this disorder. We studied 13 patients, suffering of Marfan's syndrome, with suspected aortic dilatation by means of magnetic resonance imaging (MRI). Aneurysmal dilatation of the aortic root and dissection were the two major findings in our study. Two of the five patients with dissections presented without relevant symptoms in the medical history nor at the time of the MRI examination.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Acta neurochirurgica 116 (1992), S. 44-48 
    ISSN: 0942-0940
    Keywords: Cervical discectomy ; cervical radiculopathy ; cervical myelopathy ; disc herniation ; myelography ; magnetic resonance imaging ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary In a prospective study of 63 surgical patients cervical myelography was compared with MRI to establish the relative value of the 2 diagnostic procedures in patient selection for surgery of ruptured cervical discs and bony nerve root compression. While MRI in the T1-weighted and gradient echo modes matched the diagnostic accuracy of invasive myelography (95%), T1 and T2-weighted MRI images alone were associated with an error rate of 10%. In patients with medial protrusion myelography did not always show the true extent of compression, whereas MRI tended to miss small laterally protruding disc fragments. Cervical myelography continues to have a place in the diagnosis of cervical disc disease, whenever clinical signs and symptoms do not agree with MRI data.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Acta neurochirurgica 116 (1992), S. 119-127 
    ISSN: 0942-0940
    Keywords: Arteriovenous malformation ; cavernous angioma ; MRI ; surgery
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary AVMs of the posterior fossa are reviewed on the basis of personal experience of 47 cases including 2 venous angiomas, 7 cavernous angiomas, 5 arteriovenous fistulas and 33 true arteriovenous malformations and of the few series reported in the literature. MRI is now an indispensable tool to define the exact localization of any malformation. Combined with angiography, it permits one to choose the most adequate therapeutic strategy and the best surgical approach. Radical cure is to be contemplated in most cases considering the often dramatic consequences of bleeding at the infratentorial level. Deep AVMs and moreover cavernous angiomas, even those located in highly functional structures such as the brain stem, can now be discussed for treatment. Encouraging results have already been obtained using, alone or in association, the recently advanced modalities of treatment: interventional neuroradiology, radiosurgery, and microsurgery.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 0942-0940
    Keywords: Intraparenchymal brain tumour ; malignancy ; Gd-DTPA ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The feasibility of diagnosing the malignancy and viability of intraparenchymal brain tumours using Gd-DTPA, enhanced and unenhanced T1-weighted MRIs was investigated. The relationship between the Gd-DTPA enhancement pattern, the growth fraction (GF) determined by using the anti-bromode-oxyuridine (BrdU) monoclonal antibody, the clinical condition, the proliferative potential and the change of Gd-DTPA enhancement over time was studied. Forty-five patients with intracranial tumours were studied with the static method of Gd-DTPA MRI. The enhanced effect in Gd-DTPA MRIs was dependent on tumour-cell density, vascularization, necrosis, and dilatation of vascular lumen. Tumour-cells were observed in eighty-seven of eighty-nine specimens taken from areas with Gd-DTPA enhanced MRIs. Seventy-four percent of these specimens (64 of 87) showed a malignancy of more than 5% growth fraction. On the other hand, tumour cells were observed in twentyseven of fifty-six specimens taken from areas with Gd-DTPA unenhanced MRIs. Eighty-five percent of these specimens (23 of 27) showed a malignancy value of less than 5% GF. However, fifteen percent of these specimens showed values between 5 and 15% GF. In the kinetic study of Gd-MRIs five patients who were in a clinically stable condition and one patient who had radionecrosis showed a constant pattern of enhancement or slightly increased enhancement 30 min after injection compared to 4 min after injection. Therefore, GD-DTPA MRI can be used effectively in the diagnosis of tumour viability and malignancy after treatment.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 1432-1084
    Keywords: Urinary bladder carcinoma ; Pelvis ; MRI ; Gadolinium-DTPA ; T-Staging
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Forty-nine patients with urinary bladder carcinomas underwent pre-operative examinations using magnetic resonance (MR) imaging. The results of the MR examinations were correlated with the clinical-pathological findings following transurethral resection (TUR) and bimanual palpation (n = 47) or radical cystectomy (n = 2). The results of pre-contrast MR tumor staging (T1, T2), viewing stages Tis-T2 collectively, and subsequent to separate assessments of stages T3b-T4b, were correct 76.6% of the time. Gadolinium-DTPA (Gd-DTPA) contrast-enhanced examinations (pre-contrast T1 and after Gd-DTPA) showed a staging accuracy rate of 85.7%. T2-weighted images did not indicate any advantage when compared to T1-weigthed images follwing Gd-DTPA. The signal intensity ratios of tumor/fat and tumor/muscle tissue were measured on T1-weighted pre-contrast images and following Gd-DTPA and then evaluated statistically, whereby the increased tumor signal intensity was statistically significant (Wilcoxon test, P 〈 0.01). Due to the relatively short examination time needed for T1-weighted images and the specific tumor enhancement, the administration of Gd-DTPA proves valuable in the diagnosis of bladder carcinomas. T2-weighted images are not necessary.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1432-1084
    Keywords: MRI ; Shoulder ; Fat saturation ; Gradient-echo sequences ; Soft-tissue contrast
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Although the signs of complete rotator cuff tears on MRI are well established, tendinitis and partial rotator cuff tears cannot always be readily depicted. In order to optimize the soft-tissue contrast of shoulder imaging without increasing imaging time for routine applications, we compared spin-echo and gradient-echo sequences with and without fat saturation and studied the soft-tissue contrast of spoiled gradient-echo sequences with several different parameters. We conclude, that fat-saturation is not necessary in order to improve the soft-tissue contrast. Successful fat suppression was only achieved in 50% of cases. We found a gradient-echo sequence with a double echo acquisition (echo times TE: 11 and 34 ms) with a long repetition time (TR: 600 ms) and a moderate flip angle (20°) very helpful in diagnosing rotator cuff pathology.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1432-1084
    Keywords: Induratio penis plastica (IPP) ; Peyroni'es Disease ; Ultrasound ; MRI ; Gadolinium-enhanced
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Penile induration, a disease of connective tissue, requires the precise delineation and differentiation of inflammatory changes (plaques) for accurate therapy. Seventy two patients with clinically suspected Induratio penis plastica (IPP) underwent ultrasound examination between 1984 and 1991. In 37 patients (aged 18 to 80) the diagnosis was proven by ultrasound. Out of this group 27 patients were examined with magnetic resonance imaging (MRI), 15 of them with additional intravenous application of adolinium DTPA (Gd-DTPA). All examinations were performed within four weeks. The results showed, that ultrasound was able to detect plaques and changes of the tunica albuginea in all 37 cases, but MRI was more sensitive in the detection of possible inflammatory change (T2-prolongation and moderate Gd-DTPA enhancement in gradient-echo sequences. MRI revealed inflammatory changes in 22 of 27 examined patients while ultrasound detected only nine such cases out of 37. Ultrasound is the method of choice in diagnosing IPP, due to the overall sensitivity to plaques and changes in the tunica. On the other hand MRI offers valuable additional information with respect to inflammatory changes particularly after Gd-DTPA. Therefore MRI has the potential to improve therapeutic planning and should be used in monitoring therapeutic effects.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    European radiology 2 (1992), S. 508-510 
    ISSN: 1432-1084
    Keywords: MRI ; Knee joint ; Three-dimensional reconstruction: preprocessing, segmentation, shading, surface rendering, volume rendering, hybrid rendering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract We tried to improve the basic three-dimensional reconstruction technique by comparing preprocessing, segmentation, shading and rendering techniques in 15 examples of MR investigations of the knee joint. We conclude that signal-normalising, combined threshold and tracking segmentation, grey-level-gradient shading, and combined surface and volume rendering (i. e. hybrid rendering) are the methods of choice for the three-dimensional reconstruction process.
    Type of Medium: Electronic Resource
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  • 10
    ISSN: 1432-1084
    Keywords: Diffuse liver disease ; MRI ; CT ; Ultrasound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Twenty-nine patients with diffuse liver disease were examined by ultrasound, CT and MRI. MRI was performed using T1- and T2-weighted spin-echo sequences as well as fast gradient-echo-sequences. The paramagnetic contrast agent Gd-DTPA was applied intravenously (0.1 mmol/kg). in patients with hepatitis, MRI could be used in guiding liver biopsies as inflammatory changes were clearly delineated. CT and ultrasound were superior to MRI in the detection of focal or diffuse fatty degeneration. On the other hand MRI was more helpful in differentiating fatty changes and neoplasm. In liver cirrhosis, fibrotic changes were most clearly demonstrated by MRI. In patients suffering from hemochromatosis MRI offers advantages over CT and ultrasound in the diagnosis and follow up due to the paramagnetic properties of iron, resulting in a reduction in signal intensity. In patients with Wilson's disease a characteristic pattern of parenchymal changes was seen. Administration of Gd- DTPA contributes additional information about perfusion conditions in the liver parenchyma, however this information was not of diagnostic relevance in the cases we studied.
    Type of Medium: Electronic Resource
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  • 11
    ISSN: 1432-1084
    Keywords: MRI ; Psychiatry ; white matter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract T2-weighted MRI scans of psychiatric patients with at least one white matter lesion (WML) were compared to 83 non-psychiatric controls with respect to WML number and distribution. MANOVA results in significant effects for sex, age and patient group with respect to WML number. In the psychiatric patients, infratentorial WML prevailed in organic psychoses. WML number was positively correlated with age with the exception of rith temporal lobe WML. Based on WML spatial distribution, four patient clusters were found. Clusters with widely distributed WML comprised older patients with late onset of illness; right frontal and temporal WML were associated with mania, euphoria and unstable mood.
    Type of Medium: Electronic Resource
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  • 12
    ISSN: 1432-1920
    Keywords: Multiple sclerosis ; MRI ; Mass lesions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Six patients presenting with new neurological deficits underwent magnetic resonance imaging (MRI) that displayed mass lesions leading to diagnoses of tumor or abscess. Biopsy revealed demyelinating lesions.
    Type of Medium: Electronic Resource
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  • 13
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 34 (1992), S. 105-106 
    ISSN: 1432-1920
    Keywords: syphilis ; spinal cord ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary MR imaging was performed on a patient with syphilitic myelitis. T2-weighted images showed high intensity areas in the thoracic spinal cord. On T1-weighted images after gadolinium-DTPA injection, heterogeneous enhancement was observed in the superficial portion of the spinal cord. The intramedullary high intensity areas on T2-weighted images disappeared after antibiotic therapy.
    Type of Medium: Electronic Resource
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  • 14
    ISSN: 1432-1920
    Keywords: Angioma ; Central nervous system, angioma ; MRI, spinal cord ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary We report a patient with multiple angiographically occult vascular malformations in the brain and spine. Magnetic resonance imaging showed multiple lesions in brain and spine with hypointense areas on both T1 and T2-weighted images. These hypointense areas are usually secondary to hemosiderin deposits consistent with remote bleeding in the lesions. We conclude that when magnetic resonance reveals an intraspinal lesion with signal intensity characteristics consistent with a vascular malformation, an examination of the brain should be performed to rule out associated intracranial lesions. The finding of multiple lesions in the brain with identical signal intensity characteristics reinforces the diagnosis of vascular malformation.
    Type of Medium: Electronic Resource
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  • 15
    Electronic Resource
    Electronic Resource
    Springer
    Neuroradiology 34 (1992), S. 117-121 
    ISSN: 1432-1920
    Keywords: Cockayne's syndrome ; Ataxia telangiectasia ; Fanconis anaemia ; Central nervous system ; MRI ; CT
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The CT and MRI appearances of 5 patients with Cockayne's syndrome, 5 with ataxia telangiectasia and 1 with Fanconi's anaemia are reported. These conditions, together with Bloom's syndrome and xeroderma pigmentosum are regarded as disorders of DNA repair. Characteristic CT and MRI features of Cockayne's syndrome include generalised atrophy, calcification in basal ganglia and dentate nuclei and white matter low density. Neuroradiological findings in the other DNA repair disorders are nonspecific.
    Type of Medium: Electronic Resource
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  • 16
    ISSN: 1432-1920
    Keywords: Granuloma paranasal sinuses ; Computed tomography ; MRI ; Lethal midline granuloma ; Lymphoma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary In 13 patients presenting as lethal midline granuloma (LMG), computed tomography proved essential for determining the extent of the disease, guiding biopsy and planning radiotherapy. Magnetic resonance imaging (MRI) was also helpful for the latter, because it could distinguish fluid retained within the paranasal sinuses from solid masses and tumour from granulation tissue; it was of little value for detecting bone lysis. Eight of the 13 patients proved to have T-cell lymphoma, two had Crohn's disease, in one the lesion was factitious and two had granulomas without diagnostic histological features.
    Type of Medium: Electronic Resource
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  • 17
    Electronic Resource
    Electronic Resource
    Springer
    European radiology 2 (1992), S. 2-13 
    ISSN: 1432-1084
    Keywords: Contrast media ; MRI ; Ultrasound ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
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  • 18
    Electronic Resource
    Electronic Resource
    Springer
    European journal of pediatrics 151 (1992), S. 38-41 
    ISSN: 1432-1076
    Keywords: Mediastinal cysts ; MRI ; Children
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The signals obtained from mediastinal cystic lesions in children by magnetic resonance imaging (MRI) have been analysed. The advantages and pitfalls in establishing the final diagnosis by MRI are compared to the conventional radiographic technique and to computed tomography.
    Type of Medium: Electronic Resource
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  • 19
    Electronic Resource
    Electronic Resource
    Springer
    European archives of psychiatry and clinical neuroscience 242 (1992), S. 69-71 
    ISSN: 1433-8491
    Keywords: Marchiafava-Bignami disease ; CT ; MRI ; SPECT ; Corpus callosum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Marchiafava-Bignami disease (MBD) is a rare complication of chronic alcoholism. The clinical features, X-ray, CT and MRI findings are well documented. However, functional brain imaging has not been used in cases of MBD. We used single-photon emission computed tomography (SPECT) to monitor the regional cerebral blood flow in a patient suffering from a acute form of MBD, from which he subsequently recovered. Several abnormalities were found. A more frequent use of functional brain imaging in MBD could improve our knowledge of pathogenesis and prognosis for MBD.
    Type of Medium: Electronic Resource
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  • 20
    Electronic Resource
    Electronic Resource
    Springer
    Neurological sciences 13 (1992), S. 517-519 
    ISSN: 1590-3478
    Keywords: MRI ; cerebellum ; anoxic ; ischemic encephalopathy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Sommario Un indagine di RM rivelò un quadro di alterazioni simmetriche nel putamen e negli emisferi cerebellari in una paziente sopravvissuta ad un arresto cardiorespiratorio dovuto a polineurite acuta idiopatica. Dal momento che alterazioni simili possono far seguito ad intossicazione da cianuro o da metanolo, la diagnosi differenziale di queste condizioni deve tener conto sia degli elementi clinico-anamnestici sia degli elementi della diagnostica per immagini.
    Notes: Abstract MRI demonstrated symmetric putaminal and cerebellar changes in a patient who survived a cardiorespiratory arrest due to acute idiopathic polyneuritis. Since similar aspects can be observed following cyanide or methanl poisoning differential diagnosis from these conditions has to rely on the combination of clinical and imaging findings.
    Type of Medium: Electronic Resource
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  • 21
    Electronic Resource
    Electronic Resource
    Springer
    Oral radiology 8 (1992), S. 37-43 
    ISSN: 1613-9674
    Keywords: Chondrosarcoma ; Mandibular condyle ; CT ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract A rare case of chondrosarcoma of the mandibular condyle is reported. CT and MRI were available in the diagnosis of chondrosarcoma, but plain radiograms were nearly non-contributory. Microscopically, the malignant chondroid tissue and malignant chondrocytes were observed.
    Type of Medium: Electronic Resource
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  • 22
    Electronic Resource
    Electronic Resource
    Springer
    Oral radiology 8 (1992), S. 33-39 
    ISSN: 1613-9674
    Keywords: MRI ; Gd-DTPA ; Cystic lesion ; Odontogenic tumor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The authors present examples of the significantly improved diagnostic imaging for cystic lesions in the jaw bone, floor of the mouth and maxillary sinus with Gadolinium-DTPA (Gd-DTPA) enhanced MRI. Twelve cases of cystic lesions, which were 6 cases of intra-osseous odontogenic cysts and cystic tumors, 2 cases of epidermoid cysts in the floor of the mouth and 4 cases of cystic polyp of the maxillary sinus. Improved MR images provided useful information delineating the thickness of circumscribed soft tissue wall (cystic wall), the location of the intra-cystic substance and the configuration of the tumor masses.
    Type of Medium: Electronic Resource
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  • 23
    Electronic Resource
    Electronic Resource
    Springer
    European journal of applied physiology 65 (1992), S. 438-444 
    ISSN: 1439-6327
    Keywords: Force/CSA ; Muscle stress ; Specific tension ; Skeletal muscle strength ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The physiological cross-sectional areas (CSAp) of the vastus lateralis (VL), vastus intermedius (VI), vastus medialis (VM) and rectus femoris (RF) were obtained, in vivo, from the reconstructed muscle volumes, angles of pennation and distance between tendons of six healthy male volunteers by nuclear magnetic resonance imaging (MRI). In all subjects, the isometric maximum voluntary contraction strength (MVC) was measured at the optimum angle at which peak force occurred. The MVC developed at the ankle was 746.0 (SD 141.8) N and its tendon component (F t) given by a mechanical advantage of 0.117 (SD 0.010), was 6.367 (SD 1.113) kN. To calculate the force acting along the fibres (F f) of each muscle, F t was divided by the cosine of the angle of pennation and multiplied for (CSAp · ΣCSAp−1), where ΣCSAp was the sum of CSAp of the four muscles. The resulting F f values of VL, VI, VM and RF were: 1.452 (SD 0.531) kN, 1.997 (SD 0.187) kN, 1.914 (SD 0.827) kN, and 1.601 (SD 0.306) kN, respectively. The stress of each muscle was obtained by dividing these forces for the respective CSAp which was: 6.24 × 10−3 (SD 2.54 × 10−3) m2 for VL, 8.35 × 10−3 (SD 1.17 × 10−3) m2 for VI, 6.80 × 10−3 (SD 2.66 × 10−3) m2 for VM and 6.62 × 10−3 (SD 1.21 × 10−3) m2 for RE The mean value of stress of VL, VI, VM and RF was 250 (SD 19) kN m2; this value is in good agreement with data on animal muscle and those on human parallel-fibred muscle.
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  • 24
    ISSN: 1573-7373
    Keywords: metastatic disease ; spinal cord ; MRI ; myelography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Comparison between myelography (MY) and magnetic resonance imaging (MRI) was carried out in 36 patients with clinical suspicion of spinal cord or root compression due to metastatic disease in the spinal canal. In 3 patients metastatic lesions were visualized on MY but not on MRI, while there were no cases with a negative MY and a positive MRI. In 44% of the cases MY alone or combined with postmyelographic CT (pm-CT) showed a larger tumor extension than did MRI, while the opposite occurred in 25%. As for detection of bony metastases and tumor masses localized outside the spine there was no difference between MRI and MY + pm-CT. The results indicate that the choice between MRI and MY + pm-CT still can be based on the availability and quality of the procedure at a given institution.
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  • 25
    ISSN: 1573-7373
    Keywords: CT ; irradiation ; leukoencephalopathy ; methotrexate ; MRI ; PET
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A case of treatment-related leukoencephalopathy is presented. A patient with medulloblastoma was postoperatively treated with craniospinal axis irradiation. One month after irradiation, weekly intrathecal administration of methotrexate was performed 4 times to treat cerebrospinal fluid dissemination of the tumor. Two months after the initiation of intrathecal chemotherapy, the patient became somnolent and developed decerebrate posturing. Magnetic resonance imaging showed diffuse leukoencephalopathy. Positron emission tomography revealed a diffuse decrease in glucose uptake in the deep white matter. Auditory evoked potential also showed diffuse abnormalities, not only in the cerebrum, but also in the brain stem. High dose intravenous leucovorin rescue was attempted without any neurologic improvement.
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  • 26
    Electronic Resource
    Electronic Resource
    Springer
    Brain topography 5 (1992), S. 129-133 
    ISSN: 1573-6792
    Keywords: NMR ; MRI ; MRS ; Nuclear magnetic resonance ; Brain metabolism ; Imaging ; Functional brain imaging ; Spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The first successful demonstrations of nuclear magnetic resonance (NMR) in bulk matter were reported in 1946 (Bloch, Hansen and Packard 1946; Purcell, Torrey and Pound 1946). Since then NMR has become a widespread technique for investigating matter of all kinds. In the 1970's NMR was applied to living systems, including man, in 2 distinct approaches. One application was in the production of images (Lauterbur 1973), called Magnetic Resonance Imaging or MRI, and the other in the production of NMR spectra (Moon and Richards 1973; Hoult et al. 1974), called Magnetic Resonance Spectroscopy or MRS. By appropriate manipulation of the NMR signal an NMR image may be generated. This can be a 2D image of a single slice, or a set of 2D images of parallel slices, or a 3D image. 2D images may be obtained directly in any orientation, axial, coronal, sagittal. The method uses no ionizing radiation and is inherently safe. It is non-invasive, although paramagnetic solutions may be injected intravenously to improve contrast. MRI images observed in normal clinical practice are maps of the NMR signals from water and fat in the tissues; they depend on proton density, but also significantly on the relaxation times T1 and T2. Images can be provided of flow (MR angiography) and diffusion (free, restricted or anistropic). Images are typically 512×512 pixels with spatial resolution of about 0.5mm. The images can be correlated with anatomical structures and indeed MRI is a primary source of such structures with localization precision of 0.5mm as in CT. Normal imaging times are about 5mins, but fast images of lower resolution can be obtained in 50ms, enabling real time movie images to be generated. Recording sessions are typically 1hr. The NMR spectrum from living tissue gives a non-invasive measure of the concentration of each molecular species. Such spectra (MRS) provide information concerning the biochemistry of the body's metabolism and associated pathology.31P spectra report concentrations of ATP, ADP, phosphocreatine, inorganic phosphate, other metabolites and also local pH.1H spectra (with suppression of water and lipid responses) give spectra from lactate, NAA, choline, creatine and other components. Spectroscopic Imaging (SI) combines MRI and MRS to provide spectra simultaneously from an array of pixels or voxels, each usually several cm3 in size in an overall time of order 20 mins. This procedure provides a spatial map of the whole spectrum or individual maps of each molecular species. Two recent developments have demonstrated that NMR can provide functional mapping of the normal human brain, and map the response of the human cerebral cortex to physiological stimulation.
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  • 27
    Electronic Resource
    Electronic Resource
    Springer
    Brain topography 5 (1992), S. 153-157 
    ISSN: 1573-6792
    Keywords: Brain Imaging ; CT ; Geometrical Features ; Image Matching ; Image Processing ; Image Registration ; MRI ; SPECT
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Clinical diagnosis, as well as therapy planning and evaluation, are increasingly supported by multimodal images. There are many instances desiring integration of the information obtained by various imaging devices. This paper describes a new approach to match images of different modalities. Differential operators are used in combination with Gaussian blurring to extract geometric features from the images that correspond to similar structures. The resulting ‘feature’ images may be used with existing matching techniques that minimize the distance between the features in the images to be matched. Our first application of this new approach concerns matching of MRI and CT brain images. The so-called Lυυ operator produces a ridge-like feature image from which in CT and MRI the center curve of the cranium is easily extracted. First results of this operator's performance in matching tasks are shown. Another promising operator is the ‘umbilicity’ operator, which is presented in combination with SPECT images.
    Type of Medium: Electronic Resource
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  • 28
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 20-23 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid, specific and reliable gas chromatographic assay procedure for Nifedipine in plasma has been developed. With a single-step solvent extraction, and electron capture detection, the method is sensitive to 0.5 ng/mL of plasma and the standard curve is linear from 0.5 to 500 ng/mL. Samples are protected from light to prevent formation of photodecomposition products. The method has been used to monitor drug concentrations in patients receiving therapeutic doses.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 29
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Blood group B antigenic trisaccharide-β-aminopropyl glycoside (B-TSAP) covalently attached to poly-N-(2-hydroxyethyl)acrylamide-coated porous glass interacts with anti-B monoclonal antibodies faster than the ligand coupled to CNBr-activated Sepharose 4B and Affi-Gel 10. Rates of hydrophobic adsorption of antibodies on the butyl derivatives of the same supports were measured to evaluate the diffusion input to overall kinetics. The lowest average affinity adsorption time [t1(aff) = 250 s] observed for polymer-coated glass probably arises because of the flexibility of the extended segments of chemisorbed N-substituted polyacrylamide acting as effective spacer arms.
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  • 30
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Antibodies against gangliosides isolated from small tumour and nervous tissue specimens can be reliably detected in serum samples by the ganglioside electrotransfer technique without the need for previous purification steps. After separation by high performance thin layer chromatography gangliosides are transferred from silica gel plates to hydrophobic polyvinylidene difluoride membranes. These membranes are highly suitable for immuno-staining. The use of a 15-slit device allows simulataneous testing of up to 15 serum samples. Samples of serum from 39 patients with clear-cell carcinoma of the kidney, mammary carcinoma, ovarian carcinoma and neurological disorder together with samples from healthy controls were tested for anti-ganglioside antibodies from various tissues.
    Additional Material: 4 Ill.
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  • 31
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: This paper describes a high performance liquid chromatographic (HPLC) method for determining 1,5-anhydroglucitol in plasma, in which anion exchange chromatography and pulsed amperometric detection are used. Plasma samples deproteinized with trichloroacetic acid are passed through a three-layer column packed with (1) strongly basic anion (BO3-3 form, the upper layer), (2) strongly basic anion (OH- form, the middle layer) and (3) strongly acidic cation (H+ form, the lower layer) exchange resins. 1,5-Anhydroglucitol is efficiently recovered in the flow-through fraction and interfering substances are completely removed by the column treatment. The analytical response of the method is linear with concentration to 40 mg/L, and it is possible to detect as little as 0.1 mg 1,5-anhydroglucitol per litre of plasma. Analytical recovery is between 96 and 103%, and there is good agreement between the results measured by our method and by a gas/liquid chromatographic method (r = 0.998). The method has been successfully used for the determination of very low 1,5-anhydroglucitol concentrations (〈 1 mg/L) in the plasma of diabetic patients.
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  • 32
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The peroxyoxalate chemiluminescence(CL) detection method for the evaluation of the CL intensity of malondialdehyde(MDA) condensates with seven 2-thiobarbituric acid derivatives is described. The method consists of a flow injection technique together with a CL detection system using bis(2,4,6-trichlorophenyl) oxalate(TCPO) and hydrogen peroxide as chemiluminogenic reagents. Linear correlations between CL intensity and concentration are obtained for pmol levels of condensates. Among the condensates, 1,3-diethyl-2-thiobarbituric acid(DETBA)-MDA shows the largest CL intensity. High performance liquid chromatography (HPLC)/CL detection of DETBA-MDA and 1,3-diphenyl-2-thiobarbituric acid(DPTBA)-MDA using a mixture of TCPO and hydrogen peroxide in acetonitrile as a postcolumn reagent solution is also described. The detection limits for DETBA-MDA and DPTBA-MDA are 20 and 200 fmol, respectively, per 20 μL injection at a signal-to-noise ratio of 2. This HPLC/CL detection system was applied to the defermination of MDA in rat brains by using DETBA as a fluorescent derivatizing reagent.
    Additional Material: 7 Ill.
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  • 33
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: On the basis of the heparin-like effect of phosphotungstate (PTA), we have shown that it is useful for the purification of hepatitis-B virus surface antigen (HBsAg) using heparin-Sepharose affinity chromatography. HBsAg was eluted with 0.2-0.6 M NaCl. HBsAg was also eluted with PTA at approximately 1 mM, and the HBsAg fraction thus obtained contained fewer impurities than the corresponding fraction eluted with NaCl. Moreover, PTA yielded HBsAg and hepatitis-B virus e-antigen simultaneously. PTA may specifically reduce the affinity of HBsAg for heparin as well as simply competing with heparin for an anion-binding site of HBsAg. Residual PTA in the eluate was easily decomposed by alkalization, which was useful for subsequent studies.
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  • 34
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 91-94 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The use of capillary electrophoresis for simultaneous separation and detection of the two bipyridylium herbicides, paraquat and diquat, was investigated. Both herbicides were extracted from fortified sera with disposable ODS-silica cartridges. Separation was carried out using a capillary tube (50 μm i.d., 750 mm) of fused silica containing 10 mM glycine-HCl buffer (pH 3.0), 40 mM NaCl and 20% methanol as the carrier. Paraquat and diquat were completely separated in 10 min at an applied potential of 20 kV. On-column UV monitoring allowed detection of both herbicides simultaneously. The assay sensitivity was 0.05 μg/mL (signal-to-noise ratio, 2:1), which probably increases with increase in the sample volume of serum. Analytical recovery of both herbicides added to serum was about 97% at concentrations of 0.5-2.0 μg/mL.
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  • 35
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A highly sensitive and simple reversed phase high performance liquid chromatographic (HPLC) method for the quantitative determination of free fatty acids in human serum is presented. The method is based on the direct derivatization of serum fatty acids with 6,7-dimethoxy-1-methyl-2(1H)-quinoxalinone-3-propionylcarboxylic acid hydrazide. The derivatization reaction proceeds in aqueous solution in the presence of pyridine and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide at 37°C. The resulting derivatives are separated within 75 min on a reversed phase column (YMC Pack C8) with a gradient elution of aqueous acetonitrile and detected fluorimetrically. The detection limits are 2.5-5 fmol in a 10 μL injection volume. The sensitivity permits precise determination of free fatty acids in 5 μL serum. The method is simple and is without the conventional liquid-liquid extraction steps of serum fatty acids.
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  • 36
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A highly sensitive method for the determination of N-acetylneuraminic acid in human serum and urine is investigated. This method employs high performance liquid chromatography with chemiluminescence detection. N-Acetylneuraminic acid, released by hydrochloric acid hydrolysis of serum and urine, and N-glycolylneuraminic acid (internal standard) are converted into chemiluminescent derivatives with 4,5-diaminophthalhydrazide dihydrochloride, a chemiluminescence derivatization reagent for α-keto acids. The derivatives are separated within 35 min on a reversed phase column, TSKgel ODS-120T, with isocratic elution, followed by chemiluminescence detection; the chemiluminescence is produced by the reaction of the derivatives with hydrogen peroxide in the presence of potassium hexacyanoferrate(III) in alkaline solution. The detection limit for N-acetylneuraminic acid is 9 fmol (signal-to-noise ratio = 3). This sensitivity permits precise determination of N-acetylneuraminic acid in 10 nL of serum or 50 nL of urine. The method is applied to the determination of the N-acetylneuraminic acid in human sera from normal subjects and cancer patients and in normal urine.
    Additional Material: 7 Ill.
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  • 37
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The content and dissolution rate of theophylline, diprophylline and proxyphylline from a sustained release formulation were determined by UV in situ densitometry. After separation the chromatographic zones corresponding to the spots of theophylline, diprophylline and proxyphylline on the high performance thin layer chromatographic plates were scanned in reflectance/absorbance mode at 275 nm. Quantification was performed with a second degree polynomial function over the range 40-200 ng for theophylline and 60-300 ng for diprophylline and proxyphylline. Percentages of dissolved theophylline, diprophylline and proxyphylline were monitored over 1, 3 and 6 h. The method was found to be simple, accurate, reliable, time-saving (up to 18 samples can be determined simultaneously) and low-cost.
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  • 38
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An improved method for the preparation of perbenzoylated ganglioside-derived sialic acids is described. After mild acid hydrolysis, isolation of sialic acids can be achieved by Folch partition (Method A) or by anion exchange chromatography (Method B). Perbenzoylated sialic acids were freed from benzoylation reagents by a second Folch partition. Total recoveries of both methods were found to be ≥90%, calculated from metabolically labelled gangliosides. Derivatized N-acetylneuraminic and N-glycolylneuraminic acids were separated and quantified by isocratic high performance liquid chromatography using a RP18 column as the stationary phase and methanol: water (8:2) as the mobile phase. Both sialic acids were completely separated and eluted as single peaks within 15 min, monitored by UV detection. As little as 20 ng of neuraminic acid could be detected, the detector being linear up to 5 μg tested.
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  • 39
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Two enzymes, phosphoglycerate mutase and peroxidase, were purified by using an immobilized metal ion adsorbent for the removal of unwanted proteins. The mutase was obtained pure from a single column, whereas the purification of peroxidase required the use of a thiophilic adsorbent in a tandem. The capacity was 2.5 mg pure peroxidase per mL gel.
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  • 40
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 196-197 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The separation of tetracycline and amino glycopeptide antibiotics was achieved on silica gel thin layers. Tetracycline antibiotics were resolved on a Co+2 (1.0%) impregnated silica gel layer using ethanol:acetic acid: water (10:6:6, v/v/v) as the mobile phase. Amino glycopeptide antibiotics were separated on an untreated silica gel layer using the mobile phase n-butanol: formic acid: water (6:5:7, v/v/v). The spots of these antibiotics were located by exposing the chromatoplate to iodine vapours.
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  • 41
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 212-214 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 4 Ill.
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  • 42
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    Biomedical Chromatography 6 (1992), S. 222-223 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new method for the quantification of famotidine consists of a simple extraction procedure and paired-ion high performance liquid chromatography with ultraviolet detection. The method has good accuracy and precision and should be suitable for the routine measurement of plasma and urine samples for clinical studies.
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  • 43
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    Biomedical Chromatography 6 (1992), S. 241-243 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive (1 ng/mL) and rapid method for the determination of naphazoline in rat plasma is described. Following extraction, the compound is analysed by reversed phase high performance liquid chromatography and ultraviolet detection at 214 nm.
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  • 44
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    Biomedical Chromatography 6 (1992), S. 248-250 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A procedure for the solubilization and purification of cytochrome-P450 (cyt-P450) from human liver microsomes is described. Successive treatment of microsomes with protease XXVII and 3-(3-cholamidopropyl)dimethylammoniopropanesulphonic acid gave a solubilized cyt-P450 in more than 80% yield and with a three-fold increae in specific activity. With this treatment it was possible to eliminate 80% of cytochrome-b5 and 75% of NADPH cyt-P450 reductase. The solubilized cyt-P450 was filtered on a Sephacryl-200 column and then subjected to high performance liquid chromatography with a Mono-P column (chromatofocussing). The recovery of separated cyt-P450 was about 50% with a specific activity of 11.5 nmol cyt-P450/mg protein. Also with this technique it was possible to determinate the isoelectric points of cyt-P450. These results allowed us to confirm the usefulness of our method, for the study the cyt-P450 from surgical biopsies.
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  • 45
    Electronic Resource
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992) 
    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 6 (1992), S. 255-257 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The retention behaviour of conjugated bile acids has been studied in a reversed phase high performance liquid chromatographic (RP-HPLC) system by using the mixture of methanol and aqueous phosphate buffer as the mobile phase. The retentions of the conjugates in RP-HPLC have been found to be mainly controlled by the glycine and taurine groups. The selectivity between five different glycine and taurine conjugated bile acids is a constant in RP-HPLC. This selectivity has been used for peak identification in the practical separation of conjugated bile acids.
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  • 47
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    Biomedical Chromatography 6 (1992), S. 263-263 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 48
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A combined high performance liquid chromatography/radioimmunoassay procedure is described for the simultaneous determination of dexamethasone (DEX) and its prodrug dexamethasone-21-sulphobenzoate sodium (DSS) in plasma. After precipitation of the plasma proteins by acetonitrile, the protein-free supernatant was injected onto a C18 reversed phase liquid chromatographic system and DSS- and DEX-containing fractions were collected. Hydrolysis of DSS by 0.01 N NaOH, followed by fractions extraction of both hydrolysed DSS and DEX fractions with ethyl acetate allowed the use of a dexamethasone-specific radioimmunoassay for the selective determination of both compounds. The method is accurate and reproducible (intraday variability for DSS and DEX〈6%, interday variability for DEX 14%), allowing quantification of DEX and DSS as low as 0.3 ng/mL and 0.7 ng/mL, respectively.
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  • 49
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Vaginal organic acids have previously been detected by gas-liquid chromatography, but we have applied an ion exclusion high performance liquid chromatographic procedure to the analysis of vaginal discharge samples. This procedure has the advantage of not requiring derivitization of non-volatile acids and provides the convenience of a technique which does not require the use of flammable gasses, while allowing the identification of at least 18 different acids from the same chromatographic analysis. Vaginal discharge from women with symptoms of bacterial vaginosis was collected on weighed swabs and analysed for the presence of organic acids. The results were compared to the organic acid content of samples obtained from the same cohort of women after treatment with metronidazole. In addition, samples were obtained from asymptomatic women and these samples were analysed in the same manner. The number of organic acids present in samples from women with bacterial vaginosis was greater than the number found after treatment or among asymptomatic women. Succinic acid appeared to be inversely related to lactate concentration and succinate:lactate ratios were greater among women with bacterial vaginosis before treatment than after treatment. Liquid chromatography has proven useful as a means of evaluating the metabolic end-products of vaginal microorganisms in situ.
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  • 50
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 244-247 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: CGS 18102A is a novel hexahydrobenzopyranopyridine that has a mixed pharmacological profile of 5-HT-1A agonist and 5-HT-2 antagonist properties. Based upon these mechanisms, the compound is predicted to have anxiolytic efficacy with possible efficacy in depression. Preclinical studies in the rat have shown the drug to be well absorbed and extensively metabolized. Because of the anticipated low plasma levels in humans a gas chromatography/mass spectrometry (GC/MS) analytical method has been developed and validated to determine plasma concentrations of CGS 18102A in early clinical studies. The method utilizes CGS 18416A as the internal standard. Samples (1 mL) were extracted with pentane:ethyl acetate (75:25, v:v). Extracts were then concentrated and analysed directly by GC/MS. Separation was accomplished on a methylsilicone capillary column (30 m × 0.32 mm i.d.). GC/MS was carried out under positive ion ammonia CI conditions, with selected ion monitoring of the [M + H]+ ions (m/z = 262 and 248) for CGS 18102A and CGS 18416A, respectively. The method was successively applied to the analysis of clinical samples from an ascending multidose safety and tolerability study conducted in six normal healthy male volunteers.
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  • 51
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A selective and sensitive method for the determination of low molecular weight aliphatic primary amines in urine is described. These amines were converted into their benzenesulphonyl derivatives by a modified Hinsberg procedure, and measured by gas chromatography with flame photometric detection (FPD-GC) using a DB-1 capillary column. The derivatives were very stable and provided excellent FPD responses. By FPD-GC, linear calibration curves were obtained in the range 10-200 ng of methylamine, ethylamine, n-propylamine, isobutylamine and n-butylamine using tert-butylamine as an internal standard, and the detection limits of these amines were ca. 6-25 pg as the injection amount. Benzenesulphonamide derived from ammonia was converted into its N-dimethylaminomethylene derivative which has a longer retention time, and separated from benzenesulphonyl derivatives of low molecular weight primary amines on the chromatogram. The recoveries of aliphatic primary amines added to urine samples were 91-107% and the relative standard deviations were 0.2-4.5%. Analytical results of aliphatic primary amine contents in urine samples of normal subjects are presented.
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  • 52
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992) 
    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 6 (1992), S. 269-277 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Several polymer-bound o-nitrobenzophenone reagents containing different detector-sensitive tags have been combined in the same reactor for the on-line derivatization of amine samples. The formation of multiple derivatives allows numerous opportunities for quantitation from the same injection, and also allows improved identification from the retention times of the multiple derivatives. Changing the reaction conditions changes the ratio of the products formed, so that changes in the ratio of peak heights and areas can also be used for analyte identification. In this work, propylamine was derivatized in acetonitrile on-line, precolumn. Changing the reaction conditions, of reaction time, temperature, solvent, presence of catalyst and the components of the reactor, changed the ratio of the derivatives formed. These changes in product formation with changing reaction conditions were applied to the identification and quantitation of amphetamine and methamphetamine in urine. The drugs were identified by the retention times of their derivatives, the ratio of te peak areas of the derivatives and the change in the ratios after changing reaction conditions. Each derivative was also used for quantitation of levels of spiked concentrations of amphetamine and methamphetamine, with relative errors less than 8%.
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  • 54
    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 was developed for the simultaneous assay of R(-)- and S(+)-albuterol in human serum. The assay involves solid phase extraction as a sample clean-up step and derivatization of racemic albuterol to its diastereomeric thioureas with 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl isothiocyanate. Chromatographic separation was accomplished under isocratic conditions using an octadecylsilane column and a mobile phase consisting of 29:71 acetonitrile:distilled water containing 0.1% triethylamine, pH 4.0 (adjusted with concentrated phosphoric acid) at a flow rate of 0.8 mL/min. The diastereomers were detected using a fluorescence detector set at 223 nm excitation and no emission filter. Racemic bamethane was used as internal standard. Drug to internal standard peak-height ratios were linear over a 2-20 ng/mL range for each enantiomer. The limit of detection of each analyte was 1.0 ng/mL (S/N = 3).
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  • 55
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A fully automated assay for the analysis of ranitidine in serum and plasma, with and without an internal standard, was validated. It utilizes robotic solid phase extraction with on-line high performance liquid chromatographic (HPLC) analysis. The ruggedness of the assay was demonstrated over a three-year period. A Zymark Py Technology II® robotic system was used for serial processing from initial aspiration of samples from original collection containers, to final direct injection onto the on-line HPLC system. Automated serial processing with on-line analysis provided uniform sample history and increased productivity by freeing the chemist to analyse data and perform other tasks. The solid phase extraction efficiency was 94% throughout the assay range of 10-250 ng/mL. The coefficients of variation for within- and between-day quality control samples ranged from 1 to 6% and 1 to 5%, respectively. Mean accuracy for between-day standards and quality control results ranged from 97 to 102% of the respective theoretical concentrations.
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  • 56
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    Biomedical Chromatography 6 (1992), S. 9-11 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A specific method for the determination of 10α-methoxy-9,10-dihydrolysergol, a nicergoline metabolite (metabolite 2), in urine is described. Metabolite 2 was well separated from the urine components on a reversed phase column, Hypersil ODS 5 μm, using an acetonitrile: pH 3.5 phosphate buffer (40:60, v/v) as the mobile phase at a flow rate of 1 mL/min. UV detection was set up at 220 nm. After addition of a known amount of lysergamide as the internal standard, the compounds were extracted from alkalysed urine on a pre-packed glass column (Extrelut 1) with dichloromethane. With 0.5 mL urine, concentrations down to 0.56 μmol/L could be determined.
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  • 57
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: This paper describes a method for the direct gas/liquid chromatographic (GC) analysis of 46 glycine-conjugated bile acids, which differ from one another in the number, position and configuration of the hydroxyl groups at positions C-2, C-3, C-4, C-6, C-7 and/or C-12. Free bile acids were converted quantitatively on a micro scale to ethyl ester-trimethylsilyl (Et-TMS) and methyl ester-dimethylethylsilyl (Me-DMES) ether derivatives of the corresponding glycine conjugates. The Et-TMS and Me-DMES ethers of the glycine conjugates were chromatographed on an aluminum-clad flexible fused-silica capillary column coated with a thin film (0.1 μm) of chemically bonded and cross-linked methylpolysiloxane. Relative retention time (RRT) and methylene unit (MU) values were determined for the 46 compounds and their GC behaviour was discussed. The derivatization procedure and the retention data would be useful for the direct GC identification of unknown glycine-conjugated bile acid mixtures extracted from biological samples.
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  • 58
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    Biomedical Chromatography 6 (1992), S. 24-29 
    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 the antiepileptic drug valproic acid and 14 of its metabolites in serum and urine by gas chromatography/mass spectrometry with selected ion monitoring of the trimethylsilylated derivatives has been developed. Sample preparation, including hydrolysis of VPA-conjugates and removal of urea in urine is carried out at pH 5.0 and is rapid and simple. The samples are extracted with ethyl acetate and the concentrated extracts are trimethylsilylated. Analysis with adequate separation of metabolites is achieved with a DB 1701 fused silica (Megabore) capillary column. The method exhibits high recovery and reproducibility and is sufficiently sensitive and selective for analysis of small sample volumes. Application of the method for screening patient serum and urine samples for unusual metabolite patterns, with possible predictive value for early detection of liver injury, is presented.
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  • 59
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    Biomedical Chromatography 6 (1992), S. 108-108 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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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: A high performance liquid chromatographic (HPLC) method has been developed to permit the rapid comparison of acidic polysaccharides of diverse compositions and the sensitive determination of their constituents. It is based on two combined analyses of the polysaccharide hydrolysates - a separation of the released compounds by ion-moderated partition chromatography with UV detection at two wavelengths and a separation of the sugar dansylhydrazine derivatives by reversed phase chromatography. The former permits identification and quantitation of uronic and carboxylic acids, the latter permits more sensitive and specific determination of the neutral aldoses. Some bacterial exopolysaccharides have been used to demonstrate the validity of this HPLC procedure for the chemical characterization of uronic acid-containing polysaccharides. This method appears to be useful for studying capsular polysaccharides, which are involved in the evasion of phagocytosis by pathogenic bacteria.
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  • 61
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: After inhalation experiments with sandalwood oil and the pure fragrance compounds coumarin and α-terpineol, substances were detected and measured in the blood samples of test animals (mice) using gas chromatography/mass spectrometry (GC/MS) (MID) in connection with GC/FTIR (SWC), GC/AES (carbon and oxygen trace) and flame ionization detection/gas chromatography. Using tiglinic acid benzyl ester as the internal standard the following concentrations in serum could be found: α-santalol 6.1 ng/mL, β-santalol 5.3 ng/mL and α-santalene 0.5 ng/mL. In separate inhalation experiments with coumarin and with α-terpineol the corresponding concentrations were 7.7 ng/mL and 6.9 ng/mL, respectively.
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  • 62
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A highly sensitive and simple method for the determination of prostaglandins (PGs) by HPLC with fluorescence detection is described. PGs are converted to the corresponding fluorescence derivatives by the reaction with 4-(N,N-dimethylaminosulphonyl)-7-(1-piperazinyl)-2,1,3-benzoxadiazole (DBD-PZ) in the presence of 2,2′-dipyridyl disulphide and triphenyl phosphine in acetonitrile. The reaction is completed at room temperature after 30 min. The DBD derivatives of nine PGs are separated within a single 45 min chromatographic run on a reversed phase ODS column with a linear gradient elution using water and acetonitrile. The detection limits (signal-to-noise ratio of 3) calculated from the standard mixture of PGs (6-keto-F1α, F1α, F2α, E1, E2, D2, limaprost, A1 and B1) are in the range 1.7-5.0 fmol. The applicability of the proposed procedure is evaluated to the detection of PGs added to rat plasma.
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  • 63
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    Biomedical Chromatography 6 (1992) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 64
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    Biomedical Chromatography 6 (1992), S. 183-190 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for the extraction and quantification by high performance liquid chromatography (HPLC) of non-labelled benzodiazepines partitioned into biological membranes has been developed. The benzodiazepine (BZD) was partitioned in a synaptosomal membrane-buffer system. The membranous pellet was separated by centrifugation and from this pellet, previously submitted or not to a proteolytic treatment and resuspended in the same buffer, the BZD was extracted by the addition of the proper volume of ethyl acetate, i.e. that capable of extracting at least 99.5% of the total drug in the aqueous phase. Optimal conditions for maximum proteolysis were: incubation of membranes at a final concentration of 1 mg protein/mL in the presence of 0.08 mg of Protease type I per mL for 90 min. at 45°C. Although the efficiency of the proteolysis was demonstrated not only by kinetic but also by electrophoretic evidence, recovery of BZD in the organic solvent was not increased by the enzymatic treatment at a mass BZD/protein ratio in the range 4-4.6 10-5 μg BZD/mg protein. For the HPLC quantification a reversed phase ODS column was used with methanol: water (1:1) plus 3.5% acetic acid as the mobile phase at a constant pressure and 1 mL/min flow rate. The UV detector was calibrated at 265 nm. Calibration curves were constructed by plotting peak height or peak area vs. nmoles BZD and adjusted to straight lines by a regression analysis by the least squares method. The peak height was selected as the detection method. Intra- and inter-assay precision did not exceed 10% and the total recovery was 100%.
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  • 65
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A reversed phase high performance liquid chromatographic method for the simultaneous determination of pseudouridine (PU) and creatinine (Cr) in urine is described. The mobile phase was 0.01 mol phosphate buffer (pH 6.1) containing 2.5 mmol octanesulphonic acid as the ion pairing agent. UV detection was set at 250 nm. Variation in pH value affected the retention time of PU and Cr significantly; Their separation from interfering peaks was also affected. The recoveries of PU and Cr were 89.93% and 90.35%, respectively. The standard deviation of the method for PU was 48.69 ± 0.063 (nmol/μmol Cr, mean ± SD, n = 5). The urine samples from 233 normal children of different ages and 119 patients with leukaemia were analysed by this method. The normal reference value was appraised by comparison with the percentage of immature cells in the bone marrow. The results showed that the sensitivity of the method was 94.12%, the specificity was 95.86%, the accuuracy was 95.50%, the positive predictive value was 82.05% and the negative predictive value was 98.78%. The method can be used to evaluate the state of the leukaemia, and to monitor the effect of treatment.
    Additional Material: 4 Ill.
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  • 66
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    Biomedical Chromatography 6 (1992), S. 205-211 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Zn-metallothioneins (MT-1 and MT-2) were isolated and purified from Wistar rat liver induced by subcutaneous injection with cadmium chloride over a short time. Instead of Sephadex G-50 and DEAE Sephadex A-50, new chromatographic media produced by Pharmacia, Sephacryl S-200, S-100 and DEAE Sepharose Fast Flow were used in the purification of metallothioneins. The time required for purification with the new method was only 1/3 that required with the usual method and had the same purification effect and rate of recovery. The number of mercapto groups measured with modified Ellman's reagent and cysteine as standard is 20 in MT molecules. Zn and Cd concentrations in each fraction were measured by single sweep polarography rather than atomic absorption spectrophotometry. MT-1 and MT-2 contained 6 gram atoms of zinc, but no cadmium. Purified MT-1 and MT-2 were shown by high performance liquid chromatographic analysis to be highly homogeneous and had an amino acid composition similar to that of Cd-MT.
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  • 67
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    Biomedical Chromatography 6 (1992), S. 224-226 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Haemoglobin obtained from a male adult Ghanian with retinopathy, which was probably caused by haemoglobinopathy was analysed by capillary electrophoresis (CE) for clinical diagnosis. Two major peaks, which were in the ratio of nearly one, were detected. The elution times of these peaks (HbXI and HbXII) were faster than that of normal haemoglobin (HbA). The existence of two different abnormal types of haemoglobin was clear in the patient blood. The following sequence analysis revealed that the first peak (HbXI) was HbC and the second (HbXII) was HbS on the electropherogram, and that the patient was a heterozygote of HbS and HbC (HbSC disease). One of the diagnostic processes in a haemoglobin disease was shown by the combined use of CE, HPLC and a protein sequencer.
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  • 68
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    Biomedical Chromatography 6 (1992), S. 236-240 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An analytical method has been developed for the determination of a new antiepileptic drug, CGS 18416A, in human plasma. CGS 18416A is a new anticonvulsant representative of a novel class of water-soluble agents being developed for the treatment of epilepsy. Preclinical trials indicate sustained efficacy at relatively low oral doses, indicating a need for a sensitive assay. The method is based on capillary gas chromatography/mass spectrometry and utilizes stable isotope-labelled CGS 18416A as the internal standard. Samples (1 mL) are acidified, then washed with pentane/ethyl acetate, followed by liquid/liquid extraction at pH 11 with pentane/ethyl acetate. Extracts are then concentrated and analysed directly by gas chromatography/mass spectrometry. Separation is accomplished on a thick film methylsilicone capillary column. Mass spectrometry was carried out under positive ion ammonia Cl conditions with selected ion monitoring of the protonated molecular ions (m/z = 248 and 252) for CGS 18416A and the 13CD3-CGS 18416A, respectively. Specificity was demonstrated by the lack of interfering peaks at the retention time of CGS 18416A and the internal standard. Recovery and reproducibility assessments indicate good accuracy and precision over the validated concentration range of 0.2-51 ng/mL. The limit of quantification is 0.2 ng/mL and the method has sufficient sensitivity to support clinical trials. This is illustrated with an example of quantification in a normal volunteer following oral dosing.
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  • 69
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    Biomedical Chromatography 6 (1992), S. 106-107 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 70
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    Biomedical Chromatography 6 (1992) 
    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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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive determination method for a non-fluorescent anti-arrhythmic drug, mexiletine, in rat plasma is presented utilizing a HPLC peroxyoxalate chemiluminescence (PO-CL) detection system. After an internal standard (4-methylmexiletine, 4.35 pmol) and 0.1 N sodium hydroxide solution were added to 5 μL rat plasma, the solution was poured onto an Extrelut 1 column. Both mexiletine and the internal standard were eluted with diethy ether and then the eluate was evaporated to dryness. The residue was dissolved in 0.2 M borate buffer (pH 8.5) and mixed with dansyl chloride (75 nmol) in acetronitrile. After standing of 90 min at room temperature, 0.5 N HCI was added to the reaction mixture to stop the reaction and a 2/45 aliquot of the mixture was subjected to a HPLC PO-CL detection system using bis(4-nitro-2(3,6,9-trioxadecyloxycarbonyl)phenyl)oxalate (TDPO) and hydrogen peroxide. The calibration curve for mexiletine in rat plasma was linear over the range 20-100 ng/mL plasma (20.6-103 fmol/injection). The detection limit (S/N = 2) was 1.0 fmol over the whole procedure. The method was applied to the measurement of the time courses of plasma mexiletine concentration after oral administration of the drug [25 mg (115.9 μmol)/kg] to rats.
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  • 72
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    Biomedical Chromatography 6 (1992), S. 162-162 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 73
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The increased attention on the therapeutic implications of stereoisomerism has provided an impetus for the development of analytical methods for enantiomeric separation. The indirect method of separation of enantiomers as diastereomers using high performance liquid chromatography (HPLC) has emerged as an efficient and versatile approach. This is due mainly to the availability of numerous chiral derivatization reagents (CDRs). This article reviews CDRs useful for the development of an indirect HPLC method using ultraviolet, fluoresence and electrochemical detection. In addition, factors crucial for the development of the indirect method are discussed.
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  • 74
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    Biomedical Chromatography 6 (1992), S. 194-195 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The Hageman factor fragment (HFf) concentrate was prepared from acetone and dextran sulphate activated human plasma by chromatography on a CM-Sephadex column. The preparation was free of the main kallikrein inhibitors - Cl-inactivator, α2-macroglobulin, antithrombin III and α1-antitrypsin. The HFf concentrate can serve as an activator of prekallikrein in patient plasma.
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  • 75
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    Biomedical Chromatography 6 (1992), S. 198-204 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive method for the determination of hyoscine (scopolamine) in urine is described. After concentration and “clean-up” on C18 and CN solid phase extraction columns, hyoscine was quantified by high performance liquid chromatography with coulometric detection (oxidation at +0.9 V). The limit of detection was 5 ng per sample and the precision for 5 mL samples containing 2 ng/mL was 12.3%. The method was applied to urine samples collected from 12 volunteers wearing Scopoderm TTS patches. The mean excretion rate of unmetabolized hyoscine was 0.45 μg/h and 87% of the total hyoscine was present as conjugates. Apohyoscine (aposcopolamine) was identified as a urinary metabolite. The significance of this with regard to hyoscine assays is discussed.
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  • 76
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    Biomedical Chromatography 6 (1992) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 77
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    Biomedical Chromatography 6 (1992), S. 227-230 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new method for the detection of gangliosides based on the lipophilic fluorescence agent 4-(N,N-dihexadecyl)amino-7-nitrobenz-2-oxa-1,3-diazole (NBD dihexadecylamine) and its application for preparative high performance thin layer chromatography is described. Brain gangliosides were chromatographed on silica gel coated thin layer plates and located with non-destructive fluorochrome under longwave ultraviolet light. The fluorescent zones were scraped off and the gangliosides were extracted with a mixture of chloroform/methanol/water (30/60/8; v/v/v). The gangliosides were separated from uncharged NBD dihexadecylamine by anion exchange chromatography and impurities were removed by Iatrobeads chromatography. The method described offers a simple and succesful preparative thin layer chromatographic strategy to obtain pure gangliosides in microgram and milligram quantities.
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  • 78
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    Biomedical Chromatography 6 (1992) 
    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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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A gas chromatographic/mass spectrometric procedure has been developed for the quantiation in human plasma of the enatiomers of rimanatadine and its three hydroxylated metabolites. The assay utilized derivatization of all analytes with the optically active reagent S-α-methyl-α-methoxy(pentafluorpheyl)acetic acid, selective ion monitoring, methane negative ion chemical ionization mass spectrometry and stable isotope dilution techniques. This method has been used to meausure plasma concentrations of the enantiomers of rimantadine, m-hydroxyrimantadine and p-hydroxyrimantadine (equatorial and axial epimers) in the ranges 2.5-250, 2.5-50, 1.25-62.5 and 1.25-62.5 ng/mL, respectively, in six subjects given a single 200 mg dose of racemic rimantadine. Although there are no significant differences in the concentration-time profiles of R- and S-rimantadine, large stereospecific differences in the disposition of their metabolites are observed.
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  • 80
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    Biomedical Chromatography 6 (1992), S. 53-53 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 81
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    Biomedical Chromatography 6 (1992), S. 84-87 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A universal peroxyoxalate-chemiluminescence detection system for high performance liquid chromatography, available for a variety of mobile phases, has been developed. The system consisted of a dual-head short-stroke pump and a chemiluminescence detector. The standard conditions using bis(2,4,6-trichlorophenyl) oxalate (TCPO) as aryl oxalate were as follows. The first postcolumn solution was the mixture of 0.5 M imidazole-nitric acid (pH 7.5) and acetonitrile (1:4, v/v). The second was acetonitrile containing TCPO-hydrogen peroxide. These two solutions were delivered by the two pump-heads. After the pH of the column eluate was adjusted to the optimum range (6.5-7.5) by the first postcolumn solution, the solution was mixed with the second postcolumn solution. After flowing through a reaction coil, the chemiluminescence of the mixture was monitored. Using this system, a high sensitivity (fmol level) was obtained for perylene as an analyte with mobile phases having different pH values (2.0-8.0). Polycyclic aromatic hydrocarbons became detectable to a high sensitivity even after the column separation using an acidic mobile phase. The detection sensitivity of nitrated pyrenes after on-line electrochemical reduction using an acidic mobile phase was also increased. This system might be available for other aryl oxalates by some modifications of the postcolumn solutions.
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  • 82
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    Biomedical Chromatography 6 (1992), S. 99-105 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The plasma concentrations of metoprolol enantiomers have been determined by means of a direct phenyl carbamate-cellulose-based chiral high performance liquid chromatography assay using fluorimetric detection. This assay has been used to investigate the pharmacokinetics and pharmacodynamics of metoprolol enantiomers in the conscious goat. There is evidence that the pharmacokinetics of metoprolol in the goat occurs stereoselectively and that enantiomer-enantiomer pharmacokinetic interactions occur. R-Metoprolol is less effective in reducing the mean arterial blood pressure than S- and R/S-metoprolol.
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  • 83
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    Biomedical Chromatography 6 (1992), S. 59-62 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The method for the simultaneous determination of angiotensin-converting enzyme (ACE) inhibitor enalapril and its active metabolite enalaprilat in plasma and urine was developed by gas chromatography/mass spectrometry. Enalapril and enalaprilat in plasma and urine were extracted and cleaned up by using Sep-Pak C18 and silica cartridges. Derivatization was carried out using diazomethane and trifluoroacetic anhydride. Detection by selected ion monitoring was selected to m/z 288 (enalaprilat) and 302 (enalapril). The detection limit of enalapril and enalaprilat was 200 pg/mL in plasma and 2 ng/mL in urine. This method was applied to the pharmacokinetic analysis of enalapril and enalaprilat in body fluids.
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  • 84
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A highly sensitive and selective method for the determination of spermidine and spermine has been developed. A polyamine oxidase (Aspergillus terreus) immobilized column was used as a postcolumn reactor. The detection limit was 0.2 pmol/injection for both spermidine and spermine with a linear range of three orders of magnitude.
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  • 85
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive and specific high performance liquid chromatographic method is described for measuring imidazole dipeptides and 3-methylhistidine in human muscle biopsies, serum and urine. Muscle extract, serum or urine was reacted with o-phthaldialdehyde and the derivatives were separated by reversed phase chromatography with column swithing and fluorescence detection.
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  • 86
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    Biomedical Chromatography 6 (1992), S. 35-38 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and rapid method for analysis of the core of 2′,5′-oligoadenylates, mainly based on the use of high performance liquid chromatography (HPLC), is described. Perchloric acid extracts of tissues or cells were first treated with nuclease P1. Portions of the extracts were then digested with alkaline phosphatase. HPLC analysis of the extracts was performed on a column system composed of an Ultrasphere ODS precolumn (4.6 × 45 mm) and an Ultrasphere Octyl column (4.6 × 250 mm) by stepwise elution using a 50 mM ammonium phosphate buffer, pH7, containing 3.5 and 7% methanol. Three species of the core of 2′,5′-oligoadenylates (dimer, trimer and tetramer) from a number of samples were eluted separately with 7% methanol, and the concentration of each core was directly estimated using constant values calculated with the standard core. The level of the core of 2′,5′-oligoadenylates in tissues and cells determined by our method is similar to that reported by other authors who used biological, radiobinding or radioimmunological assays.
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  • 87
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    Biomedical Chromatography 6 (1992), S. 50-52 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Orosomucoid, a member of the lipocalin family, may function in the in vivo transport of lipophilic compounds such as basic and neutral drugs. We describe the identification of 7-chloro-1-methyl-1,5-benzodiazepine-2,4-dione (clobazam) bound to the serum orosomucoid from individuals actively taking this tranquillizer. This suggests not only that other endogenous factors limit access to the benzodiazepine binding site on human serum albumin, but also that the differential binding of benzodiazepines and their metabolites by orosomucoid should be considered in determining therapeutic doses, particularly in the acute phase response.
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    Biomedical Chromatography 6 (1992), S. 278-282 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An automated analytical method utilizing laboratory robotics has been developed and validated for quantifying concentrations of a new antiepileptic drug candidate (CGP 33101) in human plasma. The robotic system aliquots the biological sample, adds the internal standard (CGP 23901) and pH 12 buffer, extracts the compounds from the basified matrix into an organic phase (methyl-t-butyl ether:dichloromethane, 2:1) and concentrates the extracts for reversed-phase, high performance liquid chromatographic (HPLC) analysis. The robotic system is directly interfaced with the HPLC system. Separation is achieved on a Hypersil 3 μm C18 column (4.6 × 50 mm) with ultraviolet detection of the analytes at 230 nm. Specificity was demonstrated by the lack of interfering peaks at the retention times for both the drug and internal standard. Recovery and reproducibility assessments indicated good accuracy (overall mean relative recovery of 102.7%) and precision (coefficient of variation of 4.4 to 7.7%) for CGP 33101 over the concentration range of 50-4000 ng/mL. The limit of quantification (LOQ) is 50 ng/mL. The method has been successfully applied to a clinical study in which normal volunteers received single oral doses of 400--1200 mg of this new drug candidate.
    Additional Material: 4 Ill.
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  • 89
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 287-290 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The technique of high performance immunoaffinity chromatography was used to measure the levels of recombinant interferon in chronic lymphocytic leukaemia patients enrolled in a phase II recombinant interferon clinical trial. The technique employed a short high pressure chromatography column packed with minute glass beads which had monoclonal antibody, directed against recombinant alpha interferon, immobilized to their surface. This system was used to measure interferon levels in a variety of different human body fluids. A good correlation was found when interferon levels, detected by chromatographic separation, were compared to levels obtained by a conventional radioimmunoassay.
    Additional Material: 3 Ill.
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  • 90
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 258-258 
    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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  • 91
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 259-262 
    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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  • 92
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 265-268 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Six estrogens - estrone, equilin, estradiol, sodium estrone sulphate, sodium equilin sulphate and sodium 17-α-dihydroequilin sulphate in dog serum were successfully separated and quantified by a high performance liquid chromatographic method developed in our laboratories. The mobile phase was optimized by studying the effects of an organic modifier (acetonitrile) and an ion pairing reagent (tetrabutylammonium hydroxide). The serum sample work-up procedure was designed to recover both conjugated and unconjugated estrogens. The optimum method involved acetonitrile to precipitate serum proteins/peptides and extract estrogens. Residues were reconstituted in 50% acetonitrile in water for injection. The detection limits for these six estrogens via UV detection ranged from 0.5 to 5 ng on-column with a signal-to-noise ratio (S/N) of 10 for a 20 μL injection and via fluorescence 0.1 ng on-column for 17-β-estradiol. Validation data are included for all six estrogens.
    Additional Material: 3 Ill.
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  • 93
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive and selective liquid chromatographic method to quantitate MDL 201,012 in human plasma was developed and validated. MDL 201,012 (I), diethyl-MDL 201,012 (internal standard, II) and desmethyldiol-MDL 201,012 (masking agent, III) were isolated from basified plasma (2 mL) by solid phase extraction using Bond-Elut® C-18 cartridges. Endogenous components were selectively removed prior to eluting the analytes from the sorbent. Components were separated using on-line LC column switching with a cyanopropyl precolumn and a phenyl analytical column. The analytical column effluent was monitored electrochemically at a glassy carbon electrode at a potential of + 1025 mV vs. Ag/AgCI. Peak-height ratios were proportional to the amount of MDL 201,012 added to plasma over the range 125-7500 pg/mL MDL 201,012. Absolute recovery of MDL 201,012 from human plasma was 〉94% across the calibration range. The minimum quantitation limit was 125 pg/mL. Assay precision (%RSD) ranged from 5.2 to 13% based on the analysis of quality control standards containing 125, 250, 500, 1000, 2500, 5000 and 7500 pg/mL MDL 201,012. Corresponding assay accuracy (% relative error) was ±8.5%. The method has been successfully used to quantitate MDL 201,012 in samples from acute dose tolerance studies in human volunteers.
    Additional Material: 3 Ill.
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  • 94
    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 for the analysis of chlortetracycline (CTC) using postcolumn fluorescence detection has been developed. After chromatographic separation of CTC on a polystyrenedivinylbenzene copolymer column, a highly fluorescent derivative isochlortetracycline (iso-CTC) was formed postcolumn in an on-line reaction coil with the addition of 25% NaOH (w/v). Chromatographic separation was achieved on a PRP-1 column, 15 cm × 4.6 mm, with 27:73 acetonitrile:0.2% perchloric acid (v/v), at 1.0 mL/min. Fluorescence derivatization was achieved by the on-line addition of 25% NaOH (w/v), at a flow rate of 0.2 mL/min, into the column eluant in a post-column reaction coil. The reaction coil was 9 m of teflon (1/16 in o.d., 0.3 mm i.d.) knitted into a six-sided coil. The fluorescent derivative was detected at λex 355 nm and λem 〉389 nm. Using this method after a simple sample cleanup, CTC can be detected in milk at 0.04 μg/mL, which is comparable to that obtained by microbiological assays. The detection method was linear between 0.02 μg/mL and 4 μg/mL. Because of the chromatographic separation, the method is more selective than microbiological assays and more sensitive than ultraviolet detection. With the chromatographic system described, the keto tautomeric forms of CTC and 4-epi-CTC are separated in a system which minimizes their formation on-column. In acidic aqueous organic solutions, the keto tautomer of CTC is the only product formed to any significant amount.
    Additional Material: 7 Ill.
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  • 95
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    Springer
    Medical & biological engineering & computing 40 (1992), S. 145-152 
    ISSN: 1741-0444
    Keywords: Brain glioma ; Classification ; Fuzzy rule extraction ; MRI
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology , Medicine
    Notes: Abstract The current pre-operative assessment of the degree of malignancy in brain glioma is based on magnetic resonance imaging (MRI) findings and clinical data. 280 cases were studied, of which 111 were high-grade malignancies and 169 were low-grade, so that regular and interpretable patterns of the relationships between glioma MRI features and the degree of malignancy could be acquired. However, as uncertainties in the data and missing values existed, a fuzzy rule extraction algorithm based on a fuzzy min-max neural network (FMMNN) was used. The performance of a multi-layer perceptron network (MLP) trained with the error back-propagation algorithm (BP), the decision tree algorithm ID3, nearest neighbour and the original fuzzy min-max neural network were also evaluated. The results showed that two fuzzy decision rules on only six features achieved an accuracy of 84.6% (89.9% for low-grade and 76.6% for high-grade cases). Investigations with the proposed algorithm revealed that age, mass effect, oedema, post-contrast enhancement, blood supply, calcification, haemorrhage and the signal intensity of the T1-weighted image were important diagnostic factors.
    Type of Medium: Electronic Resource
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  • 96
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    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 6 (1992) 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 97
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 6 (1992), S. i 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 98
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    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 6 (1992), S. 63-64 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 99
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 6 (1992), S. 65-83 
    ISSN: 0886-9383
    Keywords: Trilinear decomposition ; Receptor modeling ; Source identification ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In many cases, monitoring data for ambient airborne particles can be organized in the form of a three-way data table with one way for chemical species, one for sampling periods and one for sites. A direct trilinear decomposition followed by a matrix reconstruction (DTDMR) is developed to analyze such a data table as a whole. The three-way data set is composed into three two-way matrices by a direct trilinear decomposition (DTD). The column vectors of each of the matrices are called ‘source profiles’, ‘emission patterns’ and ‘site coefficients’ respectively. Particulate sources are identified by examining both their source profiles and emission patterns. After the sources have been identified, emission patterns and site coefficients are used to produce a three-way matrix that gives estimates of mass contributions of sources to the samples collected at every site in every period. By simulation study, not only has the method been verified, but a good indicator has been found that shows the number of factors (i.e. sources) in the system. Unlike other receptor models, DTDMR does not require source profile data and does not involve trial-and-error procedures. Since DTDMR identifies sources based on variations in two dimensions, it has a higher potential to distinguish two sources that have similar chemical compositions. The DTDMR model has provided excellent results with simulated data and has been applied in a real world three-way data set.
    Additional Material: 7 Ill.
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  • 100
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    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 6 (1992), S. 113-116 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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