固相萃取与气相色谱-质谱联用测定血清中9种有机磷残留

Solid-phase extraction coupled with GC/MS for the determination of organophosphorus pesticides in serum samples

建立了固相萃取与气相色谱-质谱(GC/MS)联用同时测定血清中9种有机磷农药的方法。样品通过C18固相萃取柱,用正己烷-二氯甲烷混合溶剂进行洗脱,经0.45μm滤膜过滤后,常温下N2吹干,加入100μL乙酸乙酯重溶,GC/MS进行测定。方法测定甲拌磷、二嗪农、氯唑磷和水胺硫磷线性范围为0.1~100μg/L,乙酰甲胺磷、灭线磷、丙溴磷和甲基嘧啶磷线性范围为0.5~100μg/L,甲基毒死蜱线性范围为1.0~100μg/L,线性相关系数(R2)均大于0.99。检出限为0.01~0.23μg/L,3根不同SPE柱日内和日间精密度分别为3.2%~8.6%和5.0~8.5%。测定血清中9种有机磷,回收率在72.7%~119.4%之间。该方法满足血清中多种有机磷农药残留的同步测定。

Solid-phase extraction coupled with GC/MS was established for the determination of 9 organophosphorus in serum samples.The mixture of 800μL serum sample and 800μL deionized water was passed through C18 solid-phase extraction column.Then the analyte on the column was eluted with 800μL and200μL mixted solvent of hexane and methylene chloride,respectively.The eluate was collected and filtered through 0.45μm filtering membrance.Then it was dried by N2 blowing and dissolved with 100μL ethyl acetate.An aliquot of 1μL was introduced to GC/MS.The linear ranges of phorate,diazinon,isazofos,isocarbophos were 0.1-100μg/L;the linear ranges of acephate,ethoprophos,profenofos,pirimiphos-methyl were 0.5-100μg/L and the linear range of chlorpyrifos-methyl was 1-100μg/L,with all the coefficents R2 higher than0.99.The limits of detection(3 S/N)were 0.01-0.23μg/L.The intra-day and inter-day precisions were3.2%-8.6%and 5.0%-8.5%,respectively.Using serum sample as the matrix,the recoveries of the 9 organophosphorus pesticides were 72.7%-119.4%.This method can satisfy the requirement for simultaneous analysis of various organophosphorus pesticides in serum.