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.%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(Ds-TDG)为内标进行定量测定.结果 方法在1～150 μg/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、0.5 μg/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.
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