کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1172462 960774 2006 7 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Liquid-phase microextraction for sample preparation in analysis of unconjugated anabolic steroids in urine
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Liquid-phase microextraction for sample preparation in analysis of unconjugated anabolic steroids in urine
چکیده انگلیسی

The applicability of in-vial two-phase liquid-phase microextraction (LPME) in porous hollow polypropylene fiber was studied for the sample preparation of unconjugated anabolic steroids in urine. Four different anabolic steroids – metabolites of fluoxymesterone, 4-chlorodehydromethyltestosterone, stanozolol and danazol – were used as test compounds and methyltestosterone as an internal standard. A standard two-phase LPME method for use with liquid chromatography/mass spectrometry (LC/MS) was set up and the influence of different parameters, including the nature of organic solvent, extraction time, salting-out and temperature, on the LPME process was investigated. Taking advantage of the preliminary studies, a novel two-phase LPME method utilizing simultaneous in-fiber silylation was developed and validated for gas chromatographic/mass spectrometric (GC/MS) analysis of a danazol metabolite in urine. In all, LPME allowed a very straightforward, simple and selective way to prepare urine samples for steroid analysis, being most suitable for hydrophobic steroids. The LPME method with in-fiber derivatization for GC/MS analysis exhibited high sensitivity, repeatability and linearity and enabled simultaneous filtration, extraction, enrichment and derivatization of the analyte from urine matrix without any other steps in sample pretreatment.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Analytica Chimica Acta - Volume 559, Issue 2, 16 February 2006, Pages 166–172
نویسندگان
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