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  • Life and Medical Sciences  (48,545)
  • Analytical Chemistry and Spectroscopy  (25,705)
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  • 1
    Electronic Resource
    Electronic Resource
    Fluorescence high performance liquid chromatographic determination of 3α-hydroxysteroids in urine of 21-hydroxylase deficiency (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 1-6 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A fluorescence high performance liquid chromatographic method using an immobilized 3α-hydroxysteroid dehydrogenase column as a post-column enzymatic reactor was developed for the determination of corticosteroid metabolites in the urine of subjects with congenital adrenal hyperplasia. 3α-Hydroxysteroids, such as pregnanetriol, pregnanediol and pregnanetriolone, in the eluate from μ-Bondapak phenyl column (300 × 3.9 mm I.D.) using 0.05% ammonium phosphate buffer (pH 7.1)-acetonitrile-methanol (100: 55: 15) as the mobile phase was mixed with NAD+ solution in the enzyme column at 30 °C to generate NADH, which was monitored by a fluorophotometric detector. Each steroid was measured at the 2.5 μg/dl at the highest sensitivity of the detector. The mean recoveries and reproducibilities were 91.5-108.2% with 0.9-6.5% (CV%).
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010102
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  • 2
    Electronic Resource
    Electronic Resource
    Measurement of urinary cystine and cysteinyl-penicillamine in patients with cystinuria (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 21-26 
    Details
    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 with electrochemical detection (LC/EC) was developed to measure cystine and cysteinyl-penicillamine disulfide in the urine of patients screened or treated for cystinuria. Urine was acidified, centrifuged to remove urinary protein, diluted and injected. The disulfides were separated on a reversed-phase column, reduced at the upstream electrode of a dual electrochemical detector with gold-mercury amalgam (Au/Hg) electrodes and the resultant thiols measured at the downstream electrode. The sample preparation is simple, the analysis rapid, specimens can be easily batched and the specificity of the method is better than those of two other separative procedures with which it was compared. The coefficient of variation for cystine in cystinuric urine is 6.7%, 5.5% and 3.2% for levels of 0.09, 0.52 and 1.02 mmol/l respectively, and for cysteinyl-penicillamine disulfide 2.6% and 7.5% for levels of 0.45 and 0.98 mmol/l respectively. Urine for analysis of these disulfides should not be collected within 24 hours of administration of the radiopaque agent diatrizoate but no other interference to the assay has been noted. This method is suitable as a screen for cystinuria in patients with renal tract calculi, for ongoing monitoring of cystinuric patients and to check patient compliance with d-penicillamine therapy.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010106
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  • 3
    Electronic Resource
    Electronic Resource
    Early identification of isovaleric aciduria using photodiode array detection for liquid chromatographic profiling of urinary carboxylic acids (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 38-40 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The 190 nm high performance liquid chromatographic photodiode array profiling of the urinary carboxylic acids of the first urine of a newborn affected with isovaleric aciduria afforded an abnormal peak at 27.8 min. This peak was greatly increased in the carboxylic acid profiling of the 14 h urine sample from the same infant. Isolation of this peak by fraction collecting; solvent extraction of the eluent; trimethylsilyl derivatization of the residue and gas chromatographic/mass spectrometric analysis identified the compound as isovalerylglycine. Correlation of the 190 nm absorbance of isovalerylglycine (y) with concentration (x) afforded a least squares curve: y = 476.4x - 13.72 (r = 0.99) run-to-run variation 6.92%; day-to-day variation 8.88%; with a minimum detectable concentration of 25 μg/ml.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010109
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  • 4
    Electronic Resource
    Electronic Resource
    Combined use of lectin affinity chromatography and endo-β-galactosidase to study polylactosamine sequences isolated from haemopoietic cell surfaces (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 41-47 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The trypsin-sensitive glycopeptides from cell surfaces of a multipotential murine haemopoietic cell line (DE) have been studied using serial lectin affinity chromatography on columns of immobilized lentil lectin (LCA), concanavalin A (Con A), and wheat-germ agglutinin (WGA). WGA-binding material consisted of glycopeptides that failed to bind to LCA and Con A. Step elution from the WGA-column with 0.01-, 0.1-, 0.5- and 1.0 M N-acetyl-D-glucosamine yielded four affinity classes of glycopeptide (WGA-W, WGA-I, WGA-S and WGA-SS respectively). WGA-W, WGA-I and WGA-S contained both alkali-stable (N-linked) and alkali-labile (O-linked) carbohydrate on high molecular weight glycopeptides. The WGA-SS fraction contained only N-linked carbohydrate. N-linked glycopeptides isolated from each WGA-binding class differed in molecular size, relative N-acetylneuraminic acid content and affinity for Ricinus communis 120 agglutinin. endo-β-Galactosidase digestion showed that these glycopeptides contained polylactosamine-type glycans. Gel filtration profiles of the enzyme treated materials were different for each WGA-binding population suggesting variation in branching patterns and/or substitution with fucose residues. Affinity chromatography has shown that the WGA binding molecules are the major glycopeptide group at DE cell surfaces.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010110
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  • 5
    Electronic Resource
    Electronic Resource
    Separation and studies of serum proteins with aid of aqueous two-phase systems containing dyes as affinity ligands (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 64-77 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 21 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010205
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  • 6
    Electronic Resource
    Electronic Resource
    Analysis of urine and faecal porphyrins by HPLC coupled to an advanced automated sample processor (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 93-94 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010208
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  • 7
    Electronic Resource
    Electronic Resource
    Paper chromatography of urinary amino acids. A 30 year survey of dietary influences on the normal pattern, and patients' results (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 95-100 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: In the clinical laboratory, paper chromatography is still the most useful, simple, inexpensive procedure for initial identification of abnormalities of amino acid excretion. The results of its use for more than 8000 paediatric and adult renal patients is surveyed. Nonspecific generalized aminoaciduria was the most frequent abnormality found, comprising some 70% of abnormal results, with cystine-lysinuria the next most common. The identification of the abnormal excretory pattern of amino acids as distinct from the normal was complicated by the effects of the New Zealand diet. In particular, valine, citrulline, hydroxyproline and glutamic acid are found in considerable amounts as part of the normal pattern. Their dietary origin is discussed. Varying mixtures of monosaccharides and disaccharides occurred in association with a range of amino acid patterns.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010302
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  • 8
    Electronic Resource
    Electronic Resource
    Use of biological fluids for the rapid diagnosis of potentially lethal inherited disorders of human purine and pyrimidine metabolism (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 109-118 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Inherited purine and pyrimidine disorders may be associated with serious, sometimes life-threatening consequences. Early and accurate diagnosis is essential. Difficulties encountered when using existing high pressure liquid chromatographic (HPLC) methods led to the development of an improved method based on prior fractionation of urine. The advantages are as follows. 1. Production of fingerprints demonstrating altered urinary excretion patterns characteristic of any one of ten different disorders, in 30 minutes. 2. Positive identification and quantification by comparison with established methods (using conventional chromatography, electrophoresis and UV spectrophotometry) in addition to specific retention times and characteristic UV absorbance ratios at two separate wavelengths (245 and 280 nm) by HPLC. 3. Direct analysis of all the purines and pyrimidines normally found in human body fluids as well as identification of abnormal compounds. 4. Short time between successive analyses while maintaining excellent resolution between compounds of interest and column longevity. 5. Improved separation of the different adenine-based compounds encountered in some disorders, plus demonstration of potential interference by dietary or drug metabolites. 6. Applicability to the monitoring of therapy involving a variety of different purine and pyrimidine analogues.Particular attention should be paid to sample preparation. Plasma profiles will confirm the diagnosis in some, but not all, of these disorders.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010305
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  • 9
    Electronic Resource
    Electronic Resource
    Measurement of penbutolol and 4-hydroxypenbutolol in plasma or serum by HPLC (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 140-142 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple HPLC method for penbutolol and 4-hydroxypenbutolol assay has been developed. Plasma or serum (200 μl) is vortex-mixed (30 s) with Tris solution (2 M, pH 10.6) containing an internal standard (50 μl) and methyl t-butyl ether (200 μl). After centrifugation, the extract (100 μl) is analysed using an unmodified silica column (250 × 5 mm ID) and iso-octane-methanol-methyl t-butyl ether (55:25:20) containing ammonium perchlorate (10 mM, pH 5.7) as eluent and with fluorescence detection. No interference has been encountered and the limit of accurate measurement for both compounds is 5 μg/l.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010309
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  • 10
    Electronic Resource
    Electronic Resource
    Metabolic profiling of opioid peptides in canine pituitary and selected brain regions using HPLC with a radioreceptor assay detector (1986)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 126-139 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A combination of gradient reversed-phase high performance liquid chromatography (RP/HPLC) with a radioreceptor assay detector that uses two ligands is used to obtain effectively the metabolic profile of endogenous receptoractive opioid peptides in the canine pituitary and in seven selected brain regions including the hypothalamus, caudate nucleus, mid-brain, amygdala, thalamus, pons-medulla, and the hippocampus. Gradient RP/HPLC separates a mixture of endogenous peptides over a wide range of hydrophobicities. A novel opioid preparation from canine limbic system synaptosomes is utilized in a radioreceptorassay screen; tritiated etorphine (ET) or D-2ala, D-5leu-leucine enkephalin (DADL) is used as the competitively displaced ligand. This receptor-rich preparation contains several receptor types, and thus serves well as a screen with the required low level of specificity. Subsequent analysis with other detectors of high specificity (MS, RIA) will follow this screen in other studies. Etorphine interacts with several of the opioid peptide-preferring receptors, whereas DADL is more specific towards the delta receptor that preferentially binds the smaller pentapeptides of the enkephalin family. The highest amount of peptide receptor activity found in this study is in the pituitary tissue, a smaller amount in the hypothalamus and caudate nucleus, and still lower amounts in the other five brain tissue extracts. This variation in peptide concentration most probably reflects three separate factors that operate in this biologic system: differential tissue-specific processing patterns of the large peptide precursors; distribution of the three opioid peptide systems; and the receptor preparation and the radioligand used in the assay. The structures of the receptoractive compounds in each RP/HPLC peak await mass spectrometric confirmation.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130010308
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