色谱法
化学
二氯甲烷
固相萃取
萃取(化学)
尿
检出限
气相色谱-质谱法
气相色谱法
基质(化学分析)
样品制备
质谱法
重氮甲烷
溶剂
有机化学
生物化学
作者
Danuta Ligocka,Dominique Lison,Vincent Haufroid
标识
DOI:10.1016/s0378-4347(01)00441-8
摘要
The aim of this work was to validate a sensitive method for quantitative analysis of 5-hydroxy-N-methylpyrrolidone (5-HNMP) in urine. This compound has been recommended as a marker for biological monitoring of N-methylpyrrolidone (NMP) exposure. Different solvents and alternative methods of extraction including liquid–liquid extraction (LLE) on Chem Elut and solid-phase extraction (SPE) on Oasis HLB columns were tested. The most efficient extraction of 5-HNMP in urine was LLE with Chem Elut columns and dichloromethane as a solvent (consistently 22% of recovery). The urinary extracts were derivatized by bis(trimethylsilyl)trifluoroacetamide and analysed by gas chromatography–mass spectrometry (GC–MS) with tetradeutered 5-HNMP as an internal standard. The detection limit of this method is 0.017 mg/l urine with an intraassay precision of 1.6–2.6%. The proposed method of extraction is simple and reproducible. Four different m/z signal ratios of TMS-5-HNMP and tetralabelled TMS-5-HNMP have been validated and could be indifferently used in case of unexpected impurities from urine matrix.
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