کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1207372 965265 2009 6 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Determination of fecal sterols by gas chromatography–mass spectrometry with solid-phase extraction and injection-port derivatization
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Determination of fecal sterols by gas chromatography–mass spectrometry with solid-phase extraction and injection-port derivatization
چکیده انگلیسی

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 0.02–10 ng/mL with coefficients of determination, R2 > 0.995. Good reproducibility was obtained with relative standard deviation less than 19.6%. The limits of detection ranged from 1.3 ng/mL to 15 ng/mL (S/N = 3) in environmental water samples. Compared with traditional off-line silylation of fecal sterols performed with water bath (60 °C, 30 min), this injection-port silylation method is much simpler and convenient. The developed method has been successfully applied for the analysis of fecal sterols from real environmental water samples.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography A - Volume 1216, Issue 7, 13 February 2009, Pages 1053–1058
نویسندگان
, , , , ,