改良QuEChERS法与LC-MS/MS联用测定水产品中13种农药残留  

Determination of 13 Pesticide Residues in Aquatic Products by Modified QuEChERs Method Coupled with LC-MS/MS Quantification

作　　者：尹怡[1] 赵城[1] 余权[2] 李丽春[1] 刘书贵[1] 单奇[1] 马丽莎[1] 郑光明[1] Yin Yi;Zhao Cheng;Yu Quan;Li Lichun;Liu Shugui;Shan Qi;Ma Lisha;Zheng Guangming(Pearl River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Minisitry of Agriculture Laboratory of Quality&Safety Risk Assessment for Aquatic Product(Guangzhou)/Key Laboratory of Recreational Fisheries Research,Ministry of Agriculture,Guangzhou 510380;Guangzhou Forensic Science Institute,Guangzhou 510030)

机构地区：[1]中国水产科学研究院珠江水产研究所/农业部水产品质量安全风险评估实验室(广州)/农业部休闲渔业重点实验室,广州510380 [2]广州市刑事科学技术研究所,广州510030

出　　处：《中国食品学报》2019年第11期255-260,共6页Journal of Chinese Institute Of Food Science and Technology

基　　金：国家自然科学基金青年科学基金项目（31501398）;国家农产品质量安全风险评估项目（GJFP2016009）;广东省省级财政专项资金项目

摘　　要：采用改良的QuEChERS方法提取与净化水产样品,建立氯嘧磺隆、异丙草胺、嘧菌酯等13种农药残留同时测定的液相色谱-串联质谱(LC-MS/MS)检测方法。样品用含1%乙酸的乙腈溶液提取,提取液用聚苯乙烯-二乙烯基苯(PS-DVB)和乙二胺-N-丙基硅烷(PSA)分散固相萃取净化,将目标物在电喷雾正离子(ESI+)电离,多反应监测(MRM)模式下测定,基质外标法定量。在优化的试验条件下,13种目标物在1~100μg/L范围内线性关系良好,相关系数均大于0.99,方法检出限为0.15~0.75μg/kg。分别对空白罗非和空白对虾按5,20μg/kg和50μg/kg等3个水平添加13种农药,目标物的平均回收率为75%~120%,相对标准偏差(RSD,n=5)均小于15%。采用该方法测定12份鱼样和18份虾样,在2份虾样中检出嘧菌酯,含量分别为58.4μg/kg和38.6μg/kg。试验结果表明,PS-DVB作为Qu EChERS分散固相吸附剂净化效果好、灵敏度高,且价格低廉,适用于水产品中农药多残留的检测。An improved QuEChERs pretreatment method of 13 pesticide residues in aquatic products by liquid chromatography/tandem mass spectrometry(LC-MS/MS)was developed.The sample was extracted by 1%acidic acetonitrile and purified by polystyrene-divinylbenzene(PS-DVB)and primary secondary amine(PSA).The analyte was ionized in the positive-ion electrospray ionization(ESI+)under multiple reaction monitoring(MRM)mode.Under optimized conditions,good linear relationship(R>0.99)was obtained in a concentration ranged from 1 to 100μg/L by external standard method,and the limits of detection were range from 0.15 to 0.75μg/kg.The recoveries of spiked aquatic product samples were found to be 75%-120%with RSDs under 15%(n=5).The method was successfully applied in 12 fish and 18 shrimp,and the azoxystrobin was found in shrimps,the contents were 58.4μg/kg and 38.6μg/kg.The results indicated that the rapid cost-effective accurate method was proved successful in the determination of pesticide residues in aquatic samples.Furthermore,the method is more commercial than other QuEChERS methods with advantage of low cost of PS-DVB.

关 键 词：农药残留 改良QuEChERS 液相色谱串联质谱 水产品 

分 类 号：R28[医药卫生—中药学]