液相色谱-串联质谱法测定21种植物源性食品中茚虫威残留  

Determination of Indoxacarb in 21 Plant-derived Foods by Liquid Chromatography Tandem Mass Spectrometry

作　　者：江泽军 石梦琪[1] 刘广洋[1] 李腾飞[1] 李永飞[1] 邵华[1] 金芬[1] 金茂俊[1] 佘永新[1] 王珊珊[1] 郑鹭飞[1] 王静[1] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,农业部农产品质量安全重点实验室,农业部农产品质量标准研究中心,北京100081

出　　处：《分析测试学报》2015年第8期867-873,共7页Journal of Instrumental Analysis

基　　金：中国农业科学院科技创新工程“农业化学污染物残留检测及行为研究”创新团队资助;农业行业标准制定项目(209)资助

摘　　要：建立了玉米、花生、核桃、大豆油、绿茶、葡萄、韭菜、香菇以及花椒等21种植物源性食品中茚虫威残留的液相色谱-串联质谱检测方法。样品经乙腈（植物油经正己烷-乙腈）提取,谷物、油料、坚果和植物油采用凝胶渗透色谱（GPC）净化,茶叶采用固相萃取（SPE）净化,水果、蔬菜、食用菌和香辛料采用N-丙基乙二胺（PSA）、十八烷基键合硅胶（C18）、石墨化碳黑（GCB）分散固相萃取剂（dSPE）净化,C18色谱柱分离,0.1%甲酸-乙腈（30∶70）作为流动相进行等度洗脱,质谱采用电喷雾正离子（ESI＋）模式电离,多离子监测模式（MRM）定性,基质标准曲线外标法定量。茚虫威的响应值与其浓度呈良好的线性关系,相关系数（r2）大于0.993。在3个加标浓度下,茚虫威的平均回收率为73.7%-115.2%,相对标准偏差不大于13.1%,方法的定量下限为1.5-9.5μg/kg,该方法可满足茚虫威残留分析的要求。A sensitive and selective liquid chromatography - positive tandem mass spectrometric （LC -MS/MS） method was developed for residue in 21 plant-derived foods, such as maize, peanut, walnut, leek, mushroom and Chinese prickly ashy. The analyte in plant oil mode electrospray ionization - the determination of indoxacarb soybean oil, green tea, grape, sample was extracted with n-hexane and acetonitrile, and the analyte in other kinds of samples was extracted by acetonitrile. Different types of samples were cleaned up by various methods. The extracts of grain, oil crops, nut and plant oil were cleaned up by gel permeation chromatography （ GPC）, the extract of tea was purified with solid-phase extraction（SPE） column, the extracts of fruits, vegetables, edible fungus and spice were cleaned up with dispersive solid-phase extraction （dSPE） sorbents, namely primary secondary amine（ PSA）, octadecylsilane（ C18 ） and graphitized carbon black（GCB）. Then indoxacarb in the extract was separated on a reversed phase C18 column using an isocratic elution program of 0. 1% formic acid-acetonitrile（30 ： 70）. Qualitative analysis was performed by electrospray ionization in positive mode（ ESI^＋） under multiple reaction monitoring （MRM） mode. The matrix-matched calibrations were used to quantify the residue concentrations. The calibration curves showed good linearities in the certain concentration range for different matrices, with correlation coefficients（ r2） more than 0. 993. The average recoveries of indoxacarb in different matrices were in the range of 73.796 - 115.2% at three spiked concentration levels, and relative standard deviations（ RSD, n = 5） were not more than 13.1%. The limits of quantitation（LOQ） were 1.5 -9. 5 μg/kg in different matrices. The method is versatile, sensitive and accurate, and could meet the detection requirements of indoxacarb residue in plant-derived foods.

关 键 词：茚虫威 液相色谱-串联质谱法 植物源性食品 

分 类 号：O657.6[理学—分析化学] S482.3[理学—化学]