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

作　　者：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] 

机构地区：[1]军事医学科学院毒物药物研究所,北京100850

出　　处：《军事医学》2013年第2期135-137,共3页Military Medical Sciences

摘　　要：目的建立定量测定人体尿液中芥子气生物标志物硫二甘醇(TDG)的同位素稀释气相色谱-串联质谱法(GC-MS/MS)。方法样品中的TDG,经过HLB柱固相萃取(SPE),五氟苯甲酰氯(PFBC)衍生化后,采用GC-MS/MS选择反应监测模式分析,以氘代硫二甘醇(D8-TDG)为内标进行定量测定。结果方法在1～150μg/L范围内线型关系良好(r=0.9997),最低检出限和定量限分别为0.1、0.5μg/L,回收率为99.5%～108.8%,相对标准偏差小于10%。结论所建方法专属性强、灵敏度高。该法曾在国际禁止化学武器组织(OPCW)举办的两次生物医学样品分析国际实验室间的盲样比对测试中,取得了良好的定性定量结果。Objective To establish a quantitative analysis method for determination of sulfur mustard biomarker thiodig- lycol （TDG） 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 chro-matography-tandem mass spectrometry （GC-MS/MS） in the selected reaction monitoring mode. The quantitative analysis was performed using deuterated Ds-thiodiglycol（Ds-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 gilL 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 ex- ercise 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 

分 类 号：R446.12[医药卫生—诊断学]