LC-MS/MS测定3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留  

Pyraclostrobin,Acetamiprid and Pyridaben Residues in Three Composite Fruit and Vegetable Juice:Determination by LC-MS/MS

作　　者：叶倩 朱富伟 万凯 黄聪灵 唐雪妹 YE Qian;ZHU Fuwei;WAN Kai;HUANG Congling;TANG Xuemei(Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences,Guangzhou 510640;Laboratory of Quality and Safety Risk Assessment of Agro-product,Guangdong Province,Guangzhou 510640;Key Laboratory of Testing and Evaluation for Agro-product Safety and Quality,Ministry of Agriculture and Rural Affairs,Guangzhou 510640)

机构地区：[1]广东省农业科学院农业质量标准与监测技术研究所,广州510640 [2]广东省农产品质量安全风险评估重点实验室,广州510640 [3]农业农村部农产品质量安全检测与评价重点实验室,广州510640

出　　处：《中国农学通报》2022年第36期146-151,共6页Chinese Agricultural Science Bulletin

基　　金：国家重点研发计划“食品中农药残留标准再评估研究”(2019YFC1605204);广东省基础与应用基础研究基金项目“基于代谢组学的农药-重金属联合毒性及分子机制研究”(2020A1515010620);公益研究与能力建设项目“广东省农产品质量安全风险评估重点实验室建设”(2019年度)(2019B121203009)。

摘　　要：为了探究目前蔬果生产中常用杀菌剂、杀虫剂、杀螨剂在复合蔬果汁中的残留情况,本研究建立了3种复合蔬果汁中吡唑醚菌酯、啶虫脒和哒螨灵残留的LC-MS/MS分析方法。选取以不同蔬果进行调和的3种复合蔬果汁为材料,采用含1%(v%)乙酸的乙腈溶液提取,以SPE-NH2柱进行净化,以C18色谱柱分离待测物,采用电喷雾离子化,正离子扫描和多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。试验结果表明:啶虫脒在5~1000μg/L,吡唑醚菌酯和哒螨灵在1~500μg/L范围内均有良好的线性关系,相关系数(R2)在0.9984以上。添加浓度为0.010、0.10和0.50 mg/kg时,3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵回收率为80.6%~113.4%;相对标准偏差(RSD)介于0.5%~9.3%之间;以最低添加浓度0.010 mg/kg为方法定量限(LOQ)。该方法快捷、简便、准确,满足复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留分析的要求。In order to explore the residues of fungicides,insecticides and acaricides,which are commonly used in fruit and vegetable planting,in composite fruit and vegetable juice,a method for the simultaneous detection of pyraclostrobin,acetamiprid and pyridaben in 3 kinds of composite fruit and vegetable juice by LC-MS/MS was developed.Three composite fruit and vegetable juice made by mixed vegetables and fruits were selected as the materials.The samples were initially extracted by acetonitrile containing 1%(v%)acetic acid,and cleaned up by SPE-NH2 column.The targets were separated on a C18 column,and detected by LC-MS/MS with ESI positive polarity multiple reactions monitoring(MRM)mode.The matrix-matched external standard calibration curves were used for quantitative analysis.The results showed that:good linear relationship appeared in 5-1000μg/L of acetamiprid and 1-500μg/L of pyraclostrobin and pyridaben.The correlation coefficients(R2)were higher than 0.9984.Under three spiked levels of 0.010,0.10 and 0.50 mg/kg,the recovery rates ranged from 80.6%to 113.4%,and the relative standard deviations(RSD)were 0.5%-9.3%.Limit of quantification(LOQ)of pyraclostrobin,acetamiprid and pyridaben were 0.010 mg/kg,which was the lowest spiked concentration.The method can meet the requirements for the determination of pyraclostrobin,acetamiprid and pyridaben residues in composite fruit and vegetable juice simultaneously,and it is quick,efficient and accurate.

关 键 词：蔬果汁 吡唑醚菌酯 啶虫脒 哒螨灵 残留 

分 类 号：S482.2[农业科学—农药学]