Separation and Detection of Bile Acid 24-Glucuronides in Human Urine by Liquid Chromatography Combined with Electrospray Ionization Mass Spectrometry.
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- IKEGAWA Shigeo
- Graduate School of Pharmaceutical Sciences, Tohoku University
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- OKUYAMA Hiroko
- Graduate School of Pharmaceutical Sciences, Tohoku University
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- OOHASHI Junji
- Graduate School of Pharmaceutical Sciences, Tohoku University
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- MURAO Naoaki
- Graduate School of Pharmaceutical Sciences, Tohoku University
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- GOTO Junichi
- Graduate School of Pharmaceutical Sciences, Tohoku University
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Abstract
A method for the separation and determination of bile acid 24-glucuronides using liquid chromatography (LC)/electro-spray ionization (ESI)-mass spectrometry (MS) has been developed. In the ESI mode, 24-glucuronides were characterized by an intense deprotonated molecule [M-H]- with a fragment ion [M-H-176]- formed by elimination of the glucuronic acid moiety. The ratio of these negative ions was significantly influenced by the orifice-1 and the ring lens voltages. Bile acid 24-glucuronides in human urine were extracted with an OASIS HLB cartridge and then subjected to the LC/ESI-MS analysis employing an 18O-labeled internal standard. The simultaneous separation was attained on a Develosil ODS-HG-5 column using 20 mM ammonium acetate (pH 6.0)-acetonitrile (3:1→3:2, v/v, 35 min) in a linear gradient elution mode, where the 24-glucuronides were monitored with a characteristic negative ion [M-H]-; the limit of detection was 10 fmol. This newly developed method was applied to the quantitation of bile acid 24-glucuronides in human urine with satisfactory selectivity and reliability.
Journal
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- Analytical Sciences
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Analytical Sciences 15 (7), 625-631, 1999
The Japan Society for Analytical Chemistry
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Details 詳細情報について
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- CRID
- 1390001204257683840
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- NII Article ID
- 130004440107
- 30013459750
- 10004706652
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- NII Book ID
- AA10500785
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- COI
- 1:CAS:528:DyaK1MXks1Wqs7c%3D
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- ISSN
- 13482246
- 09106340
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- NDL BIB ID
- 4784081
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- Web Site
- http://id.ndl.go.jp/bib/4784081
- https://ndlsearch.ndl.go.jp/books/R000000004-I4784081
- https://link.springer.com/content/pdf/10.2116/analsci.15.625.pdf
- https://link.springer.com/article/10.2116/analsci.15.625/fulltext.html
- http://www.jstage.jst.go.jp/article/analsci/15/7/15_7_625/_pdf
- https://search.jamas.or.jp/link/ui/1999248964
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- Text Lang
- en
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- Data Source
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- JaLC
- NDL
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- CiNii Articles
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- Abstract License Flag
- Disallowed