高效液相-质谱联用法测定浙贝母中12种农药残留成分  

Determination of 12 kinds of pesticide residues in Fritiliariae Thunbergii Bulbus by HPLC-MS

作　　者：马临科 李文庭 赵维良 

机构地区：[1]浙江省食品药品检验研究院,浙江杭州310004

出　　处：《中草药》2014年第6期849-853,共5页Chinese Traditional and Herbal Drugs

基　　金：国家药典委员会研究基金(1677)

摘　　要：目的建立N-丙基乙二胺（PSA）-高效液相-三重四极杆串联质谱（HPLC-QQQ-MS／MS）法测定浙贝母中有机磷等12种农药残留的方法，并收集主产地浙江等地20批浙贝母样品进行农药残留测定。方法浙贝母样品加乙腈提取，过PSA柱净化，采用LC-QQQ-MS／MS方法在多反应监测（MRM）模式下测定，内标法定量。结果12种农药成分在相应的测定范围内线性关系良好，相关系数在0．9986～0．9998，12种农药在90、300、900ng／mL3个添加水平下，加样回收率范围为68．1％～108．0％，RSD为1．1％～6．1％，各农药的检出限在0．08～1．0μg／kg。结论该方法可应用于浙贝母药材中12种农药残留成分的同时检测。浙贝母药材农药残留量甚微，符合安全性要求。Objective To develop an analysis method based on N-propylethylenediamine （PSA）-HPLC-QQQ-MS/MS for the determination of 12 kinds pesticide residues in Fritiliariae Thunbergii Bulbus and to quantify them in 20 batches ofFritiliariae Thunbergii Bulbus produced in various places in Zhejiang province. Methods Fritiliariae Thunbergii Bulbus samples were extracted with acetonitrile and purified by the small column of PSA. The prepared samples were analyzed by HPLC-QQQ-MS/MS in multiple reaction monitoring （MRM） mode, and the pesticides were qualitified by the internal standard method. Results All the 12 pesticides showed good linearities in their reasonable range （r = 0.998 6--0.999 8）, and the average recoveries of all the pesticides were in the range of 68.1%-- 108.0% at three spiked levels of 90, 300, and 900 ng/mL. The RSD values were in the range of 1.1%--6.1%, and the LODs of each pesticide were all in the range of 0.08-- 1.0 I.tg/kg. Conclusion The method is suitable for the multiresidues analysis of pesticides in Fritiliariae Thunbergii Bulbus simultaneously and the quality of Fritiliariae Thunbergii Bulbus is basically good for the safty although it contains a trace of several pesticide residues.

关 键 词：浙贝母 农药残留 N-丙基乙二胺 HPLC-QQQ—MS MS多反应监测 

分 类 号：R286.022[医药卫生—中药学]