同位素稀释-气相色谱串联质谱法测定饲料中指示性多氯联苯  

Determination of Ultratrace Indicator Polychlorinated Biphenyls in Animal Feed by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Isotope Internal Standards

作　　者：王瑞国[1] 张苏[1] 董姝君 魏书林[1] 张天姝 杨浩森 程劼[1] 王培龙[1] 苏晓鸥[1] WANG Rui-Guo;ZHANG Su;DONG Shu-Jun;WEI Shu-Lin;ZHANG Tian-Shu;YANG Hao-Sen;CHENG Jie;WANG Pei-Long;SU Xiao-Ou(Institute of Quality Standards and Testing Technology for Agricultural Products,Chinese Academy of Agricultural Science, Key Laboratory of Agrifood Safety and Quality,Ministry of Agriculture,Beijing 100081,China;Liaoning Provincial Veterinary Medicine Feed Animal Product Quality and Safety Testing Center,Shenyang 110016,China)

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研究重点实验室,北京100081 [2]辽宁省兽药饲料畜产品质量安全检测中心,沈阳110016

出　　处：《分析化学》2018年第12期2019-2024,共6页Chinese Journal of Analytical Chemistry

基　　金：国家重点研发计划项目(No.2017YFC1600300);上海市科技兴农重点攻关项目(沪农科攻字(2016)第3-1号);中国农业科学院基本科研业务费专项(No.1610072018006)资助~~

摘　　要：建立了气相色谱-串联质谱法(GC-MS/MS)测定动物饲料中6种指示性多氯联苯的痕量分析方法。样品中的多氯联苯经溶剂加速萃取,用44%酸性硅胶柱脱脂和复合硅胶柱净化,气相色谱-串联质谱法分析。采用DB-5MS毛细管柱分离,电子轰击电离源(EI)电离,多反应监测模式下(MRM)检测,同位素稀释法进行定量分析。结果表明,方法的线性范围为0.1～500.0 ng/m L,相关系数(R^2)均大于0.999,平均相对响应因子(RRF)为1.08～1.21;定量限为5.5～9.2 pg/g,样品添加回收率为92.8%～109.7%,RSD为1.6%～14.8%;定量内标的回收率为32.6%～90.2%。应用此方法对北京市周边地区采集的10个配合饲料样品进行检测,6种指示性PCBs均有检出,其中PCB28和PCB52为优势单体,总浓度范围为54.7～191.7 pg/g,远低于我国国标饲料限量标准(10μg/kg)。A method was developed for determination of 6 kinds of indictor polychlorinated biphenyls in animal feed by chromatography-tandem mass spectrometry(GC-MS/MS).Analytical procedure consisted of accelerate solvent extraction(ASE),lipid removal with 44% acidic silica and clean-up using a column packed with multilayer silica.The analytes were separated on a DB-5MS capillary column,detected with electron ionization(EI)and multiple reaction monitor mode(MRM),and quantified using isotope dilution technique.The result showed that the calibration curves with good correlation coefficients(R^2>0.999)were obtained in the concentration range of 0.1-500.0 ng/mL.The average relative response factors of PCBs in calibration solvent were 1.08-1.21,and the limit of quantification were 5.5-9.2 pg/g.The average recoveries of PCBs in animal feed at two spiked concentration levels ranged from 92.8%to 109.7%with relative standard deviations(RSDs)of 1.6%-14.8%(n=5),and the average recoveries of quantitative internal standards were 32.6%-90.2%.Then the proposed method was successfully applied to detect the compound feed samples from the surrounding area of Beijing,and it was found that the 6 kinds of indictor PCBs were detected in all samples(n=10)with the total concentration ranges of 54.7-191.7 pg/g,which were far below the limit standard(10μg/kg)of Chinese National Standards.

关 键 词：指示性多氯联苯 饲料 气相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] S816.17[理学—化学]