GC-MS/MS快速测定水质中32种有机磷农药残留

Rapid determination of 32 organophosphorus pesticide residue in water by GC-MS/MS

本文建立了地表水、地下水、废水和海水中32种有机磷农药残留的测定方法。采用三氯甲烷对水样中的有机磷进行萃取,萃取液浓缩至1mL后进行GC-MS/MS分析,内标法定量。针对颜色较深的废水,以石墨化炭黑(GCB)为净化剂结合QuEChERS技术对萃取液进行净化,取得了良好的效果。实验从萃取次数和基质效应两方面对过程效率进行优化,比较了不同溶剂的提取效果。结果表明,32种有机磷农药残留在50~1000μg·L^(-1)范围内线性关系良好,线性系数R^(2)均大于0.995;地表水、地下水和海水的检出限为2.4~26.1ng·L^(-1),定量限为9.6~104.3ng·L^(-1);废水的检出限为38~236ng·L^(-1),定量限为152~945ng·L^(-1);在不同添加水平下,32种有机磷在4种水质中的回收率在65.5%~118.2%之间,相对标准偏差均小于10%。

A method for the determination of 32 organophosphorus pesticide residue in surface water,groundwater,wastewater and seawater was established.Trichloromethane was used to extract organophosphorus from water samples.The extract was concentrated to 1 mL and then analyzed by GC-MS/MS.The internal standard method was used for quantification.For the dark-colored wastewater,graphitized carbon black(GCB)was used as a purifying agent combined with QuEChERS technique to purify the extract solution,and good results were obtained.The experiment optimized the process efficiency in terms of extraction times and matrix effects,and compared the extraction effects of different solvents.The results showed that 32 kinds of organophosphorus pesticide residue had a good linear relationship in the range of 50~1000μg·L^(-1),and the linear coefficients R^(2) were all greater than 0.995.The detection limits of surface water,groundwater and seawater were 2.4~26.1ng·L^(-1),and the quantification limits were 9.6~104.3ng·L^(-1).The detection limit of wastewater was 38~236ng·L^(-1),and the quantification limit was 152~945ng·L^(-1).Under different addition levels,the recoveries of 32 kinds of organophosphorus in the four water quality ranged from 65.5%to 118.2%,and the relative standard deviations were all less than 10%.