QuEChERS-高效液相色谱-串联质谱法测定水稻中氯虫苯甲酰胺和噻虫胺的残留  

Chlorantraniliprole and Clothianidin Residues in Rice:Determined by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孙悦萍 周芹[1,3,4] 徐利剑 任红波[2] 马文琼 张晓波 金海涛 陈国峰 刘峰 董见南 SUN Yueping;ZHOU Qin;XU Lijian;REN Hongbo;MA Wenqiong;ZHANG Xiaobo;JIN Haitao;CHEN Guofeng;LIU Feng;DONG Jiannan(College of Modern Agricultural Ecology and Environment of Heilongjiang University,Harbin 150080;Safety and Quality Institute of Agricultural Products,Heilongjiang Academy of Agricultural Sciences,Harbin 150086;Beet Quality Supervision,Inspection and Test Center,Ministry of Agriculture and Rural Affairs,Harbin 150080;Laboratory of Quality Safety Risk Assessment for Sugar Crops Products,Ministry of Agriculture and Rural Affairs,Harbin 150080)

机构地区：[1]黑龙江大学现代农业与生态环境学院,哈尔滨150080 [2]黑龙江省农业科学院农产品质量安全研究所,哈尔滨150086 [3]农业农村部甜菜品质监督检验测试中心,哈尔滨150080 [4]农业农村部糖料产品质量安全风险评估实验室,哈尔滨150080

出　　处：《中国农学通报》2022年第36期126-131,共6页Chinese Agricultural Science Bulletin

基　　金：《农药产品中有效成分测定通用分析方法-液相色谱法》体系建设“啶磺草胺等10个农药品种液相色谱分析方法建立”(14192195);现代农业产业技术体系建设项目“质量安全与营养品质评价”(CARS-170503)。

摘　　要：为了监测水稻中氯虫苯甲酰胺和噻虫胺的残留量,本文建立了分散固相萃取的QuEChERS法结合超高效液相色谱串联质(UPLC-MS/MS)同时测定糙米、稻壳、秸秆中氯虫苯甲酰胺和噻虫胺残留量的测定方法。样品经乙腈水振荡提取,PSA或C18净化,UPLC-MS/MS多反应离子监测模式(MRM)下检测,外标法定量。结果表明:氯虫苯甲酰胺和噻虫胺最佳提取溶剂为50%乙腈水,提取方式为振荡提取,选择C18作为糙米提取液的净化剂,PSA作为稻壳和秸秆提取溶剂的净化剂。氯虫苯甲酰胺在0.1~100μg/L、噻虫胺胺在0.1~500μg/L范围内线性关系良好,相关系数R2均大于0.99;两种农药在糙米、稻壳和秸秆中的平均添加回收率在83.2%~105.4%之间,相对标准偏差为1.2%~10.1%;氯虫苯甲酰胺和噻虫胺在糙米中定量限为0.005 mg/kg,在稻壳和秸秆中均为0.025 mg/kg。该方法前处理过程操作简单快速,灵敏度高,适用于同时检测糙米、稻壳、秸秆中氯虫苯甲酰胺和噻虫胺的残留量。To monitor chlorantraniliprole and clothianidin residues in rice,a QuEChERS method based on dispersive solid-phase extraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for the simultaneous determination of chlorantraniliprole and clothianidin residues in brown rice,rice husk and straw.The samples were extracted by shaking with acetonitrile water solution,purified by PSA or C18,detected under UPLC-MS/MS multiple-reaction monitoring mode,and quantified by external standard method.The results showed that the best extraction solvent for chlorantraniliprole and clothianidin was 50%acetonitrile water solution,and the extraction method was shaking extraction.C18 was selected as the purifying agent for the brown rice extract,and PSA was used as the purifying agent for the extraction solvent of rice husk and straw.Good linear relations were obtained in the range of 0.1-100μg/L for chlorantraniliprole and in the range of 0.1-500μg/L for clothianidin,and the correlation coefficient R2 was greater than 0.99.The average recovery of the two pesticides in brown rice,rice husk and straw were between 83.2%and 105.4%,and the relative standard deviations were between 1.2%and 10.1%.The limit of quantitation of chlorantraniliprole and clothianidin in brown rice was 0.005 mg/kg,and the limit of quantitation in rice husk and straw were 0.025 mg/kg.The pretreatment process of the method is simple,rapid and highly sensitive.The method is suitable for the simultaneous detection of chlorantraniliprole and clothianidin residues in brown rice,rice husk,and straw.

关 键 词：氯虫苯甲酰胺 噻虫胺 分散固相萃取 高效液相色谱-串联质谱 水稻 

分 类 号：S1[农业科学—农业基础科学]