黄芪中禁用农药残留检测研究

Deternination Research of Prohibited Pesticide Residues in Astragali Radix

目的:建立黄芪中33种禁用农药的检测方法,并测定82份黄芪的禁用农药。方法:以乙腈为溶剂,高速匀浆处理,通过净化管净化。分别采用气相色谱-质谱(GC-MS/MS)法和超高效液相色谱-串联质谱(LC-MS/MS)法进行测定,正离子模式下多反应检测(MRM)。结果:GC-MS/MS法和LC-MS/MS法检测的禁用农药质量浓度在相应浓度范围内均呈良好线性关系,相关系数在0.99以上,加标回收率在59.72%~133.48%,RSD均小于13.61%,符合痕量测定的要求。82批黄芪样品共检出6批含有甲基异柳磷,检出率7.3%。结论:该方法能准确、有效检测黄芪中的禁用农药,为黄芪的安全性质量评价奠定基础,同时,为黄芪规范化种植提供依据。

Objective:To establish a detection method for 33 prohibited pesticides in Astragali Radix and determine these prohibited pesticides in 82 samples of Astragali Radix.Methods:Sample was extracted with acetonitrile and tackled with high-speed homogenization,and further purified through a purification tube.Gas chromatography-mass spectrometry(GC-MS/MS)and ultra-high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)with multi-reaction detection(MRM)in positive ion mode were used for determination,respectively.Results:The mass concentrations of detected prohibited pesticides showed a good relationship within the corresponding concentration range by GC-MS/MS and LC-MS/MS methods that the correlation coefficient was over 0.99.The recovery rate were between 59.72%and 133.48%,and the relative standard deviation was all less than 13.61%,the result indicated that conformed the requirements for trace determination.A total of 6 batches in 82 batches of Astragali Radix were detected isofenphos-methyl,the detection rate was 7.3%.Conclusion:This method can detect accurately and effectively prohibited pesticides in Astragali Radix,and provide the foundation for the safety and quality evaluation of Astragali Radix,meanwhile,it will provide a basis for standardized cultivation of Astragali Radix.