分散固相萃取-气相色谱-串联质谱法同时测定母乳中24种有机氯类农药

Simultaneous determination of 24 kinds of organochlorine pesticides in breast milk by dispersive solid-phase extraction-gas chromatography-tandem mass spectrometry

目的建立液液萃取-分散固相萃取-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定母乳中24种有机氯类农药的分析方法。方法母乳样品用正己烷-丙酮(3:1,V:V)超声提取,提取液冷冻除脂后经N-丙基乙二胺(primary secondary amine,PSA)作为分散固相萃取剂净化,净化液氮吹复溶后采用GC-MS/MS检测,内标法定量。结果24种有机氯农药在考察的浓度范围内线性关系良好,相关系数r 2≥0.99;方法检出限为0.002~0.500μg/kg,定量限为0.006~1.500μg/kg;24种目标物在高中低3个不同加标浓度下的回收率为87.1%~129.0%,相对标准偏差为1.9%~13.9%。结论该方法操作便捷、定量准确、灵敏度高,能够满足母乳样品中24种有机氯农药残留的快速检测分析需求,为监测母乳及婴儿体内的有机氯农药含量提供方法学参考。

Objective To establish an analytical method for the simultaneous determination of 24 kinds of organochlorine pesticides in breast milk by liquid-liquid extraction-dispersed solid-phase extraction-gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods Breast milk samples were extracted by ultrasound with n-hexane-acetone(3:1,V:V),the extraction liquid was frozen to remove fat,and then purified by primary secondary amine(PSA)as a dispersed solid phase extraction agent.The purified liquid nitrogen was blown and redissolved,and then detected by GC-MS/MS,and quantified by internal standard method.Results The linear relationships of the 24 kinds of organochlorine pesticides were good within the investigated concentration ranges,and the correlation coefficients r2 were all equal or greater than 0.99;the limits of detection were 0.002-0.500μg/kg,and the limits of quantitation were 0.006-1.500μg/kg;the recoveries of the 24 kinds of analytes at the 3 spiked concentrations were 87.1%-129.0%and the relative standard deviations were 1.9%-13.9%.Conclusion This method is convenient,accurate and sensitive,and can meet the requirements of rapid detection and analysis of 24 kinds of organochlorine pesticide residues in breast milk samples,providing methodological reference for monitoring the content of organochlorine pesticides in breast milk and infants.