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A method for the simultaneous analysis of unconjugated and glycine-conjugated bile acids by capillary gas-liquid chromatography

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Lipids

Abstract

A method for the simultaneous analysis of unconjugated and glycine-conjugated bile acids by means of capillary gas-liquid chromatography without need for prior deconjugation is described. The method involves: i) the use of an aluminum-clad fused-silica capillary column coated with a very thin film (0.1 μm) of a highly thermostable bonded and crosslinked methyl polysiloxane, and ii) the analysis of the bile acids as their methyl ester-dimethylethylsilyl ether derivatives. This method, used to separate the major free and glycine-conjugated bile acids from human gall bladder bile, should be applicable for the analysis of other biological fluids.

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Abbreviations

CA:

3α,7α,12α-trihydroxy-5β-cholanoic acid

CDCA:

3α,7α-dihydroxy-5β-cholanoic acid

DCA:

3α,12α-dihydroxy-5β-cholanoic acid

DMESI:

N-dimethylethylsilylimidazole

EEDQ:

N-ethoxycarbonyl-2-ethoxy-1,2-dihydroquinoline

GC:

gas-liquid chromatography

GC-MS:

gas-liquid chromatography-mass spectrometry

HDCA:

3α,6α-dihyroxy-5β-cholanoic acid

HFIP-TFA:

hexafluoroisopropyl ester-trifluoroacetyl

LCA:

3α-hydroxy-5β-cholanoic acid

Me-DMES:

methyl ester-dimethylethylsilyl

Me-TFA:

methyl ester-trifluoroacetyl

Me-TMS:

methyl estertrimethylsilyl

TLC:

thin-layer chromatography

TMS-HT:

hexamethyldisilazane and trimethylchlorosilane in anhydrous pyridine solution

UDCA:

3α,7β-dihydroxy-5β-cholanoic acid

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Authors and Affiliations

  1. College of Engineering, Nihon University, 963, Koriyama, Fukushima-ken, Japan

    Takashi Iida, Takako Itoh & Kayoko Hagiwara

  2. Department of Chemistry, Harvey Mudd College, Claremont, CA, 91711

    Frederic C. Chang

  3. Pharmaceutical Institute, Tohoku University, Aobayama, 980, Sendai, Japan

    Junichi Goto & Toshio Nambara

Authors
  1. Takashi Iida
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  2. Takako Itoh
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  3. Kayoko Hagiwara
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  4. Frederic C. Chang
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  5. Junichi Goto
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  6. Toshio Nambara
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Iida, T., Itoh, T., Hagiwara, K. et al. A method for the simultaneous analysis of unconjugated and glycine-conjugated bile acids by capillary gas-liquid chromatography. Lipids 24, 1053–1055 (1989). https://doi.org/10.1007/BF02544079

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  • DOI: https://doi.org/10.1007/BF02544079

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