Determination of fecal sterols by gas chromatography-mass spectrometry with solid-phase extraction and injection-port derivatization

Journal of Chromatography. a
Jingming WuLifeng Zhang

Abstract

Injection-port derivatization combined with solid-phase extraction (SPE) was developed and applied for the first time to determine five types of fecal sterols (coprostanol, cholestanol, epicholestanol, epicoprostanol and cholesterol) with gas chromatography-mass spectrometry (GC-MS). In this method, silylation of fecal sterols was performed with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) at GC injection-port. The factors influential to this technique such as injection-port temperature, purge-off time, derivatization reagent (BSTFA) volume, and the type of organic solvent were investigated. In addition, the conditions of SPE (including the type of SPE cartridge, the type of elution organic solvent) were also studied. After SPE followed by injection-port silylation by GC-MS, good linearity of analytes was achieved in the range of 0.02-10ng/mL with coefficients of determination, R(2)>0.995. Good reproducibility was obtained with relative standard deviation less than 19.6%. The limits of detection ranged from 1.3ng/mL to 15ng/mL (S/N=3) in environmental water samples. Compared with traditional off-line silylation of fecal sterols performed with water bath (60 degrees C, 30min), this injection-port silylation method is much s...Continue Reading

References

Dec 13, 2002·Rapid Communications in Mass Spectrometry : RCM·Wang-Hsien Ding, Cheng-Che Chiang

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Citations

Sep 8, 2015·Analytical and Bioanalytical Chemistry·Dario BattistelCarlo Barbante
Dec 6, 2011·The Science of the Total Environment·Christian G Daughton
Sep 8, 2017·Lipids·María Cuevas-TenaMaría Jesús Lagarda

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