衍生化-气相色谱-质谱法测定人体尿液中2-硫代噻唑烷-4-羧酸
摘要
人体尿液中的2-硫代噻唑烷-4-羧酸在甲醇和吡啶的催化下与氯甲酸丙酯发生反应,衍生产物经三氯甲烷液液萃取,经HP-5色谱柱分离后,进入质谱分析,以选择离子监测模式(SIM)进行测定。2-硫代噻唑烷-4-羧酸在0.05～10.0 mg/L的浓度范围内呈良好的线性关系,相关系数>0.999,方法检出限为0.01 mg/L,定量下限为0.03 mg/L;批内精密度为2.74%～3.60%,批间精密度为2.36%～3.98%;样品加标回收率为95.0%～97.5%,可以满足二硫化碳接触者尿液中2-硫代噻唑烷-4-羧酸的检测要求。
引文
[1]WS/T40—1996,尿中2-硫代噻唑烷-4-羧酸的高效液相色谱法 [S].
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[2]Husek,Simek.Alkyl chloroformates in sample derivatization strategies for GC analysis [J].Curr Pharm Anal,2006(2):23-43.
[3]Vilas-Boas SG,Delcado DG.Simultaneous analysis of amino and nonamino organic acid as methyl chloroformate derivatives using gas chromatography-mass spectrometry [J].Anal Biochem,2003,322(1):134-138.
[4]Kaspar H,Dettmer K.Automated GC-MS analysis of free amino acids in biological fluids [J].Chromatography B,2008,870(2):222-232.