气相色谱-离子阱二级质谱对照高分辨质谱对食品中二噁英类多氯联苯的测定  

Gas Chromatography-Ion Trap Tandem Mass Spectrometry versus High Resolution Mass Spectrometry for the Determination of Dioxin-like Polychlorinated Biphenyls in Food

作　　者：丁罡斗[1] 李翔[1] 仲维科[1] 张垚[1] 孙毅之[1] 刘汉霞[1] 陈彦长[1] 王大宁[1] 

机构地区：[1]中国检验检疫科学研究院

出　　处：《分析测试学报》2008年第5期479-483,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20475051);国家质检总局课题资助项目(2006IK156)

摘　　要：确定了气相色谱-离子阱二级质谱在分析食品中12种二噁英类多氯联苯残留的定性参数；优化了分析过程的质谱条件；研究了实际样品（河豚、鳗鱼、甜虾、鸡脂肪、奶粉、猪肠衣）离子阱串联质谱测定值与高分辨质谱值的准确度差异。样品采用加速溶剂萃取方法提取、流体控制系统净化及离子阱二级质谱和高分辨质谱测定。两种方法测定值之间的回归方程和相关系数分别为：4种非邻位取代二噁英类多氯联苯，y=0．7815x，r=0．9331；8种邻位取代二噁英类多氯联苯，y=0．8073x，r=0．996；样品中12种多氯联苯总毒性当量（Total TEQ）：y=0．5181x＋0．1255，r=0．992。离子阱二级质谱和高分辨质谱的检出限分别为0．5ng/kg和0．1ng／kg，样品中同位素内标的回收率为41％～102％。The qualitative parameters of gas chromatography - ion trap tandem mass spectrometry （GC -IT- MS/MS） for the determination of the residues of 12 dioxin-like polycholorinated biphenyls in food samples and the optimum operating conditions for IT - MS/MS were established. The target PCBs were extracted from the samples by accelerated solvent extraction and purified by fluid control system. The analytical results of the target PCBs in food samples（ fugu, eel, shrimp, chicken fat, milk powder, hog Casing） obtained by IT -MS/MS and high resolution mass spectrometry（HRMS） were compared in terms of variance in accuracy. The results showed that the coefficients of determination, r between the data of IT - MS/MS and HRMS for 8 ortho-PCBs, and 4 non-ortho-PCBs were O. 996 and 0. 933 1, respectively ; and the r between the toxicity equivalent obtained by IT - MS/MS and HRMS was 0. 992 for all the target PCBs. The detection limits of IT - MS/MS and HRMS were 0. 5 ng/kg and 0. 1 ng/kg, respectively. The recoveries of labeled compound solution in samples were obtained from 41% to 102%.

关 键 词：多氯联苯 气相色谱-离子阱二级质谱 高分辨质谱 食品 

分 类 号：O657.63[理学—分析化学] F407.82[理学—化学]