尿中亚硫基二乙酸测定的气相色谱-质谱法

Determination of thiodiglycolic acid in urine with gas chromatography-mass spectrometer

目的 建立氯乙烯（VCM）生物标志物亚硫基二乙酸（TDGA）的气质联用仪（GC-MS）快速检测方法.方法 以温和新型甲酯化反应替代剧毒重氮甲酯化反应,并建立高灵敏度检测方法.结果 该方法标准曲线回归线性方程：y=8 460.5x-4758.2,线性系数为0.999 7,最低定量浓度2.0 μg/L,精密度为0.81％～2.38％,平均加标回收率为99.0％～102.9％.结论 该方法降低了传统甲酯化反应的风险,较气相色谱-火焰光度检测器（GC-FPD）法提高了检测灵敏度,满足亚硫基二乙酸的检测要求.

Objective To establish a rapid determination method with gas chromatography-mass spectrometer （GC-MS） for thiodiglycolic acid （TDGA）,a vinyl chloride （VCM） biomarker.Methods A high-sensitivity determination method was established using a moderate methyl esterification instead of methyl esterification of highly toxic diazo reaction.Results The standard curve regression linear equation of the method was：y=8460.5x-4758.2,the linear coefficient was 0.999 7,the minimum quantity concentration was 2.0 μg/L,the range of precision value was 0.81%～2.38%,and the average recovery of standard addition was 99.0%～ 102.9%.Conclusion This method reduces the risk of traditional methyl esterification,improves the determination sensitivity compared with the GC-FPD method,and meets the determination requirement of TDGA.