气相色谱-串联质谱法快速筛查测定中药材中144种农药残留  

Rapid screening and quantitative analysis of 144 pesticide residues in traditional Chinese medicinal herbs by gas chromatography-tandem mass spectrometry

作　　者：程志[1] 张蓉[2] 刘韦华[2] 王金花[2] 王明林[1] 

机构地区：[1]山东农业大学食品科学与工程学院,山东泰安271000 [2]北京出入境检验检疫局技术中心,北京100026

出　　处：《色谱》2014年第1期57-68,共12页Chinese Journal of Chromatography

基　　金：国家质检总局科技计划项目(2013IK143)

摘　　要：利用气相色谱-串联质谱（GC—MS／MS）检测技术，采用QuEChERS法作为样品前处理方法，建立了能应用于11种叶J药材中144种农药残留的检测方法。探究了样品前处理过程中提取溶剂、缓冲盐体系、净化剂组成和用量对样晶提取、净化等方面的影响，最终确定了用乙腈提取，甲苯复溶，以混合净化剂净化，过有机膜后经GC-MS／MS测定，外标法定鼙。144种农药在10～2000μg／kg之间线性关系良好，相关系数（r2〉0．983；除乙酰甲胺磷、灭虫威、西玛津、克菌丹、异狄氏剂、异菌脲外，其余农药的定量限（LOQ）均低于20μg／kg；在20、50、200μg／kg的添加水平下，除乙酰甲胺磷、艾氏剂和双甲脒回收率偏低外，其余141种农药的平均回收率在74．3％～111．8％之间，相对标准偏差（RSD）为0．5％～14．6％。与已有的标准方法对比，此方法不仅检测结果一致，而且高效、快速，准确性好，灵敏度高，适用于中药材中144种农药残留的快速筛查与定量分析。An analytical method for the simultaneous determination of 144 pesticide residues in traditional Chinese medicinal herbs was established based on optimized QuEChERS with gas chromatography-tandem mass spectrometry （GC-MS/MS）. The influences of different extrac- tion solvents, different buffer systems and different purifying agents on the recoveries of the pesticides were investigated. The pesticide residues in the samples were extracted with acetoni- trile, then cleaned-up by mixed sorbents and analyzed by GC-MS/MS in multi-reaction monito- ring （MRM） mode. The external standard method was applied to quantify the pesticides. The linear range of the method was from 20 to 2 000μg/kg with the correlation coefficients （ r2 ） of more than 0. 983. The recoveries of the pesticides at the spiked levels of 20, 50 and 200μg/kg ranged from 74.3% to 111.8% with the relative standard deviations lower than 15%, except for acephate, amitraz and aldrin. The method was successfully used for the analysis of target pesti- cides in testing samples, and had a good consistency in results with the existed standard one. This multi-residue analytical method allows for a rapid, efficient, sensitive and reliable screen- ing and quantitative analysis of the target pesticides in traditional Chinese medicinal herbs.

关 键 词：QUECHERS 气相色谱-串联质谱 农药多残留 中药材 

分 类 号：O658[理学—分析化学]