建立了水样中毒死蜱及其主要代谢产物3,5,6-三氯吡啶醇(TCP)的固相萃取—气相色谱质谱检测法,即采用固相萃取对水样中的毒死蜱及其代谢产物TCP进行富集,浓缩后经双(三甲基硅烷基)三氯乙酰胺(BSTFA)衍生TCP,采用气相色谱质谱进行测定。同时,采用外标法对毒死蜱和TCP进行定量。结果表明,该方法的线性范围为20-1 000μg/L,毒死蜱和TCP的检出限分别为0.375、0.100μg/L;环境水样中的毒死蜱和TCP平均加标回收率分别为89.12%-93.44%和87.37%-90.75%,相对标准偏差(RSD)为2.79%-6.64%和1.22%-5.48%。
A method of solid phase extraction(SPE)coupled with gas chromatography-mass spectrometry(GCMS)was developed for determination of chlorpyrifos and its metabolite 3,5,6-trichloropyridinol(TCP)in water samples.SPE was firstly applied to concentrate chlorpyrifos and TCP,followed by derivatization of TCP using N,O-Bis(trimethylsilyl)trifluoroacetamide(BSTFA).The detection limits of chlorpyrifos and TCP were 0.375,0.100μg/L,recovery rates were 89.12%-93.44% and 87.37%-90.75%,relative standard deviations(RSD)were 2.79%-6.64%and 1.22%-5.48%,respectively,with a linear range from 20 to 1 000μg/L.