| Determination of 3-oxo-delta4- and 3-oxo-delta4,6-bile acids and related compounds in biological fluids of infants with cholestasis by gas chromatography-mass spectrometry. | |
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MedLine Citation:
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PMID: 9200514 Owner: NLM Status: MEDLINE |
Abstract/OtherAbstract:
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A method has been developed for the determination of 3-oxo-delta4- and 3-oxo-delta4,6-bile acids and related bile acids in biological fluids of infants by gas chromatography-mass spectrometry (GC-MS) of the methyl ester-dimethylethylsilyl ether-methoxime derivatives. The 7alpha-hydroxylated 3-oxo-delta4-bile acids were partially dehydrated to give the 3-oxo-delta4,6-bile acids by trimethylsilyl or dimethylethylsilyl derivatization and other pretreatments under acidic or alkaline conditions for GC-MS analysis. To prevent dehydration, the 3-oxo-delta4-bile acids were derivatized to the oximes by treatment with O-methylhydroxylamine prior to pretreatments such as solid-phase extraction, enzymatic solvolysis and hydrolysis of the conjugates, and silylation with dimethylethylsilylimidazole. Calibration curves for the bile acids were linear over a range of 5-250 ng and the detection limit was 100 pg for each 3-oxo-delta4-bile acid. Recoveries of the bile acids and their glycine and taurine conjugates from bile acid-free urine and serum ranged from 94.2 to 105.9% of their added amounts. The bile acids in urine and serum of four patients with severe cholestatic liver disease were measured by the analytical method, and the 3-oxo-delta4-bile acids were determined to be the major bile acids (59-68%) in the urines associated with 3-oxo-delta4-steroid 5beta-reductase deficiency or dysfunction. |
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Authors:
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M Suzuki; T Murai; T Yoshimura; A Kimura; T Kurosawa; M Tohma |
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Publication Detail:
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Type: Journal Article; Research Support, Non-U.S. Gov't |
Journal Detail:
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Title: Journal of chromatography. B, Biomedical sciences and applications Volume: 693 ISSN: 1387-2273 ISO Abbreviation: J. Chromatogr. B Biomed. Sci. Appl. Publication Date: 1997 May |
Date Detail:
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Created Date: 1997-08-20 Completed Date: 1997-08-20 Revised Date: 2006-11-15 |
Medline Journal Info:
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Nlm Unique ID: 9714109 Medline TA: J Chromatogr B Biomed Sci Appl Country: NETHERLANDS |
Other Details:
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Languages: eng Pagination: 11-21 Citation Subset: IM |
Affiliation:
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Faculty of Pharmaceutical Sciences, Health Sciences University of Hokkaido, Ishikari-Tobetsu, Japan. |
Export Citation:
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APA/MLA Format Download EndNote Download BibTex |
| MeSH Terms | |
Descriptor/Qualifier:
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Bile Acids and Salts
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blood*,
urine* Cholestasis / blood*, urine* Gas Chromatography-Mass Spectrometry Humans Infant |
| Chemical | |
Reg. No./Substance:
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0/Bile Acids and Salts |
From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine
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