气相色谱-质谱法测定小麦中二噁英类多氯联苯  

Determination of dioxin-like polychlorinated biphenyls in wheat by gas chromatography-mass spectrometry

作　　者：杨代凤[1] 刘腾飞[1] 陆皓茜[1] 毛健[1] 钱辉[1] 赵佳昕 YANG Dai-Feng;LIU Teng-Fei;LU Hao-Qian;MAO Jian;QIAN Hui;ZHAO Jia-Xin(Jiangsu Taihu Area Institute of Agricultural Sciences,Suzhou 215155,China)

机构地区：[1]江苏太湖地区农业科学研究所,苏州215155

出　　处：《食品安全质量检测学报》2020年第17期6209-6215,共7页Journal of Food Safety and Quality

基　　金：国家农业基础性长期性科技项目(ZX10S1108);苏州市科技计划项目(SNG2018055)。

摘　　要：目的建立气相色谱-质谱法(Gas chromatograph-mass spectrometry,GC-MS)同时快速测定小麦中12种二噁英类多氯联苯(dioxin-like polychlorinated biphenyls,DL-PCBs)的分析方法。方法样品采用改进的QuEChERS方法,经丙酮-正己烷(1:2,V:V)溶液超声提取,羧基化多壁碳纳米管和N-丙基乙二胺混合净化剂净化,用Agilent HP-5MS色谱柱分离,GC-MS选择离子监测模式进行测定,外标法定量。结果12种DL-PCBs在5~500μg/L范围内具有良好的线性关系,相关系数r均大于0.999。方法的检出限为0.5~0.8μg/kg,定量限均为5μg/kg,在5、10、100μg/kg添加水平的平均回收率为88.6%~115.0%,相对标准偏差小于6.5%(n=5)。结论该方法样品前处理简单快速,溶剂消耗少,对检测条件要求低,适用于同时测定小麦中12种DL-PCBs。Objective To establish a simple and rapid method for the simultaneous determination of 12 dioxin-like polychlorinated biphenyls(DL-PCBs)in wheat by gas chromatography-mass spectrometry(GC–MS).Methods The wheat samples were ultrasonically extracted with acetone-hexane(1:2,V:V).Subsequently,the extract was cleaned-up by using carboxylated multi-walled carbon nanotubes and primary secondary amine as adsorbents according to the method of QuEChERS.Then,the DL-PCBs in the extract were separated on an Agilent HP-5 MS capillary column,detected by GC-MS using selected ion monitoring mode,and quantified by external standard method.Results Good linear relationships for all the analytes were observed in the concentration range of 5–500μg/L with correlation coefficients more than 0.995.The limits of detection and the limits of quantification were 0.5–0.8μg/kg and 5μg/kg,respectively,the recoveries were ranged from 88.6%to 115.0%for the analytes with 3 spiked levels of 5,10 and 100μg/kg,and the relative standard deviations were less than 6.5%(n=5).Conclusion The proposed method is simple,accurate,solvent saving and without special instrument sensitive,which is suitable for detecting DL-PCBs in wheat.

关 键 词：二噁英类多氯联苯 小麦 气相色谱-质谱法 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]