滤过型净化柱净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定草鱼中11种农药残留  

Determination of 11 pesticides residues in grass carp using ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry coupled with pass-through clean-up column

作　　者：封腾望 王新新 周锐东 刘欢[2,3] 孙慧武 李晋成[2,3] FENG Tengwang;WANG Xinxin;ZHOU Ruidong;LIU Huan;SUN Huiwu;LI Jincheng(College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306,China;Chinese Academy of Fishery Sciences,Beijing 100141,China;Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture and Rural Affairs,Beijing 100141,China)

机构地区：[1]上海海洋大学水产与生命学院,上海201306 [2]中国水产科学研究院,北京100141 [3]农业农村部水产品质量安全控制重点实验室,北京100141

出　　处：《农药学学报》2022年第5期1268-1277,共10页Chinese Journal of Pesticide Science

基　　金：中央级公益性科研院所基本科研业务费(2020B005);中国水产科学研究院科技创新项目(2020TD75).

摘　　要：采用推杆式滤过型净化柱净化,结合超高效液相色谱-三重四极杆/复合线性离子阱质谱仪(UPLC-QTRAP-MS/MS)建立了草鱼样品中11种农药残留的检测方法。以乙腈为提取剂,样品经超声、冷冻、离心后,上清液采用以50 mg PSA为净化填料的推杆式滤过型净化柱进行1次快速净化;超高效液相色谱快速分离,三重四极杆/复合线性离子阱质谱仪进行测定。基质匹配法制作标准曲线,外标法定量。结果表明:11种农药在1.0~50.0μg/kg内的线性关系良好,相关系数均大于0.99;定量限为1.0~2.0μg/kg。不同添加水平下的回收率为83%~119%,日内相对标准偏差为2.6%~20%,日间相对标准偏差为0.7%~15%。该方法经济、简便、高效,灵敏度高,重复性好,可作为草鱼中农药残留的日常检测方法。A method was established for determination of 11 pesticide residues in grass carp sample based on cheap analytical filtration syringe(CAFS)clean-up column coupled with ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry(UPLC-QTRAP-MS/MS).Using acetonitrile as extraction solvent,the sample was ultrasonic,frozen and centrifuged,and the supernatant was quickly purified once by CAFS clean-up column with 50 mg PSA.After separated by UPLC,the analytes were determined by QTRAP-MS/MS.Matrix-matched calibration curves and the external standard method was employed for quantification.The results showed that the linear relationships of the 11 pesticides were good within 1.0-50.0μg/kg,and the correlation coefficients were greater than 0.99.The limit of quantification were 1.0-2.0μg/kg.The recoveries of 11 pesticides at different spiking levels were 83%-119%,and the intra-day and inter-day relative standard deviations were 2.6%-20%and 0.7%-15%,respectively.The method is economical,simple,efficient,sensitive and reproducible,and could be used as a routine method for the detection of pesticide residues in grass carp.

关 键 词：推杆式滤过型净化柱 超高效液相色谱-串联质谱 草鱼 农药多残留 

分 类 号：TQ450.2[化学工程—农药化工] O657.63[理学—分析化学]