加速溶剂萃取-气相色谱-串联质谱法测定水产品中的苯并(a)芘  

Determination of benzo(a) pyrene in aquatic products by accelerated solvent extraction-gas chromatography-tandem mass spectrometry

作　　者：吴金浩[1,2] 张玉凤 杜静[1,2] 李楠 王召会[1,2] 宋伦 田甲申[1,2] WU Jin-hao;ZHANG Yu-feng;DU Jing;LI Nan;WANG Zhao-hui;SONG Lun;TIAN Jia-shen(Liaoning Ocean and Fishery Science Research Institute,Dalian 116023,China;Liaoning Ocean Environment Monitoring Station,Dalian 116023,China)

机构地区：[1]辽宁省海洋水产科学研究院,辽宁大连116023 [2]辽宁省海洋环境监测总站,辽宁大连116023

出　　处：《化学研究与应用》2018年第12期2051-2056,共6页Chemical Research and Application

基　　金：辽宁省自然科学基金指导计划(201602409)资助;辽宁省海洋渔业厅科研计划项目(201303)资助

摘　　要：本文采用加速溶剂萃取技术进行样品前处理,通过对萃取溶剂、萃取温度、静态萃取时间的选择以及质谱条件的优化,研究建立了气相色谱-串联质谱法测定水产品中的苯并(a)芘的残留。结果表明:苯并(a)芘在2. 0～100. 0μg·L-1的标准曲线范围内线性关系良好,相关系数为0. 9994,方法检出限为0. 056 ng·g-1(干重),最低定量限为0. 18 ng·g-1(干重);两种添加量样品加标回收率平均值分别为93%和94%,相对标准偏差为12%和10%(n=7),该方法的准确度和精密度良好。二级质谱可有效排除水产品复杂基质的干扰,对实际水产品样品的测定也取得了较为满意的结果,本方法适合水产品中苯并(a)芘的痕量分析。The accelerated solvent extraction was used to pretreat the samples. The extraction solvent,extraction temperature,static extraction time and mass spectrum conditions were optimized.A method of gas chromatography coupled with triple quadrupole mass spectrometry( GC-MS/MS) was established for the determination of benzo( a) pyrene in aquatic products.The linear range of benzo( a) pyrene was in the range of 2. 0 μg·L^-1 and 100. 0 μg·L^-1. The correlation coefficient was 0. 9994,the detection limit of the method was 0. 056 ng·g-1( dry weight),and the lowest quantitative limit was 0. 18 ng·g-1( dry weight). The average recoveries of two different addition samples were 93%and 94%,and the relative standard deviations were 12%and 10%( n = 7). The accuracy and precision of the method were good.The second-order mass spectrometry could effectively eliminate the interference from the complex matrix of aquatic products.The method was suitable for the trace analysis of benzo( a) pyrene in aquatic products.

关 键 词：加速溶剂萃取 气相色谱-串联质谱 水产品 苯并(A)芘 

分 类 号：O657.6[理学—分析化学]