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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
引用本文:程志,张蓉,刘韦华,王金花,王明林.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[J].色谱,2014,32(1):57-68.
作者姓名:程志  张蓉  刘韦华  王金花  王明林
作者单位: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
基金项目: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种中药材中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品提取、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,外标法定量。144种农药在10~2 000μg/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。

关 键 词:QuEChERS  气相色谱-串联质谱  农药多残留  中药材
收稿时间:2013-09-26

Rapid screening and quantitative analysis of 144 pesticide residues in traditional Chinese medicinal herbs by gas chromatography-tandem mass spectrometry
CHENG Zhi;ZHANG Rong;LIU Weihua;WANG Jinhua;WANG Minglin.Rapid screening and quantitative analysis of 144 pesticide residues in traditional Chinese medicinal herbs by gas chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2014,32(1):57-68.
Authors:CHENG Zhi;ZHANG Rong;LIU Weihua;WANG Jinhua;WANG Minglin
Institution:1. College of Food Science and Engineering, Shandong Agriculture University, Tai''an 271000, China;
2. Technology Center, Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China
Abstract: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 extraction 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 acetonitrile, then cleaned-up by mixed sorbents and analyzed by GC-MS/MS in multi-reaction monitoring (MRM) mode. The external standard method was applied to quantify the pesticides. The linear range of the method was from 20 to 2000 μg/kg with the correlation coefficients (r2) of more than 0.983. The recoveries of the pesticides at the spiked levels of 20, 50 and 200 μg/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 pesticides 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 screening and quantitative analysis of the target pesticides in traditional Chinese medicinal herbs.
Keywords:QuEChERS  gas chromatography-tandem mass spectrometry (GC-MS/MS)  multi-residue pesticides  traditional Chinese medicinal herbs
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