气相色谱-串联质谱法测定稻米中毒死蜱及其代谢物  

GC-MS/MS Determination of Chlorpyrifos and Its Metabolite in Rice

作　　者：张文童[1,2] 李锐[2] 章虎[1,2] 钱鸣蓉[2] 吴俐勤[2] 王鸣华[1] 王强[2] 

机构地区：[1]南京农业大学植物保护学院农药学系,南京210095 [2]农业部农药残留检测重点实验室浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《理化检验（化学分册）》2012年第6期667-670,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江省重大科技专项(2011C12024)

摘　　要：提出了气相色谱-串联质谱法测定稻米中毒死蜱及其代谢物3,5,6-三氯-2-羟基吡啶(TCP)含量的方法。样品经含体积分数为1%盐酸的乙腈提取,盐析并浓缩至近干后,残渣用乙酸乙酯溶解TCP用N-甲基-N-叔丁基二甲基硅基三氟乙酰胺衍生化,用气相色谱-串联质谱法测定,外标法定量。毒死蜱及TCP的质量浓度与峰面积均在0.02～0.4mg.L-1范围呈线性关系,测定下限(10S/N)依次为0.5,0.2μg.kg-1。在3个浓度水平下进行了回收和精密度试验,毒死蜱和TCP的回收率分别在94.3%～111.9%和95.1%～109.6%范围内,相对标准偏差(n=5)分别在1.7%～4.0%和3.1%～11.6%范围内。GC MS/MS was applied to the determination of chlorpyrifos and its metabolite 3,5,6-trichloro-2- hydroxy pyridine （TCP） in rice. Samples were extracted with acetonitrile which contained （φ） 1% HC1. The extract was treated by salting out and evaporated to near-dryness and the residue and dissolved with ethyl acetate. TCP was derivatized with N-methybN tert-butyl trimethylsilyl trifluoroacetamide, and the derivatized product and chlorpyrifos were determined by GC- MS/MS. External standard calibration was adopted in the determination. I.inear relationships between peak areas and mass concentrations of chlorpyrifos and TCP were obtained in the same range of 0.02-0.4mg·L^-1. Values of lower limit of determination （lOS/N）were0.5,0.2μg·kg^-1 for chlorpyrifos and 0. 2 /xg ~ kg i for TCP. Tests for recovery and precision were made by standard addition method at 3 different concentration levels, values of recovery found were in the ranges of94.3%-111.9% and 95.1%-109.6%with values of RSD＇s （n=5） in the ranges of 1.7%-4.0% and 3.1%-11.6% for chlorpyrifos and TCP respectively.

关 键 词：气相色谱-串联质谱法 稻米 毒死蜱 3 5 6-三氯-2-羟基吡啶 

分 类 号：O657.63[理学—分析化学]