军事医学2013，Vol.37Issue(2)：135-137,3.DOI:10.7644/j.issn.1674-9960.2013.02.013
同位素稀释气相色谱-串联质谱法定量测定人体尿液中的硫二甘醇
A method for quantification of sulfur mustard biomarker thiodiglycol in human urine by isotope dilution gas chromatography-tandem mass spectrometry
冯建林 1白海红 1林缨 1陈佳 1刘勤 1李春正 1唐吉军 1吴弼东 1谢剑炜1
作者信息
- 1. 军事医学科学院毒物药物研究所,北京100850
- 折叠
摘要
Abstract
Objective To establish a quantitative analysis method for determination of sulfur mustard biomarker thiodiglycol (TDC) in human urine. Methods The analyte was purified and concentrated from urine on an HLB solid phase extraction (SPE) cartridge, derivatized with pentafluorobenzoyl chloride(PFBC), and analyzed by isotope dilution gas chromatography-tandem mass spectrometry ( GC-MS/MS) in the selected reaction monitoring mode. The quantitative analysis was performed using deuterated D8-thiodiglycol (Dg-TDG) as the internal standard. Results A good linear relationship was obtained within the quantitative concentration range of 1 to 150 g/L (r = 0.9997 ). The limit of detection ( LOD) and the limit of quantification (LOQ) of TDG in urine were 0.1 g/L and 0.5 g/L, respectively. The recovery for TDG ranged from 99.5% to 108.8% in urine with RSD less than 10%. Conclusion Such an GC-MS/MS established for the detection of TDG in human urine is highly specific and sensitive. The method is used in the first and the second confidence building exercise for biomedical sample analysis organized by the Organisation for the Prohibition of Chemical Weapons (OPCW) and all quantitative results of TDG are very close to the actual spiking levels.关键词
硫二甘醇/同位素稀释/气相色谱-串联质谱/固相萃取/生物医学样品Key words
thiodiglycol/isotope dilution/GC-MS/MS/solid phase extraction/biomedical samples分类
生物科学引用本文复制引用
冯建林,白海红,林缨,陈佳,刘勤,李春正,唐吉军,吴弼东,谢剑炜..同位素稀释气相色谱-串联质谱法定量测定人体尿液中的硫二甘醇[J].军事医学,2013,37(2):135-137,3.
