同位素稀释-气相色谱-三重四极杆串联质谱法测定植物油中的多环芳烃  

Determination of Polycyclic Aromatic Hydrocarbons(PAHs) in Vegetable Oil by Gas Chromatography Coupled with Triple Quadrupole Mass Spectrometry Using Isotope Dilution

作　　者：杨君[1,2] 王建华[2] 宫萍[2] 刘靖靖[2] 

机构地区：[1]青岛大学化学化工与环境学院,山东青岛266071 [2]山东出入境检验检疫局,山东青岛266002

出　　处：《食品科学》2013年第22期202-207,共6页Food Science

基　　金：国家质检总局科技计划项目(2011IK222)

摘　　要：建立凝胶渗透色谱（GPC）净化、气相色谱-三重四极杆串联质谱（GC—MS—MS）同时测定植物油中16种多环芳烃（PAHs）残留的分析方法。植物油样品加入同位素内标混合溶液后经乙腈-丙酮（60：40，V／V）混合溶液提取、GPC净化，GC-MS—MS采用选择反应监测模式（SRM）采集数据后进行分析；同时比较GPC净化和固相萃取（SPE）净化的效果，研究仪器工作条件对分析结果的影响。采用内标法定量，植物油样品中添加量为4-6μg／kg的标准品，添加回收率在70．8％～123．1％之间，相对标准偏差为1．0％～6．5％，方法的定量限为0．22～0．74μg／kg，相关系数均大于或等于0．9982。该方法适用于植物油中16种PAHs的检测。An analytical method for the determination of 16 types of polycyclic aromatic hydrocarbons （PAHs） in vegetable oil has been developed. Samples that had been spiked with isotope standard solution were extracted using acetonitrile/ac- etone （60：40, V/V） and purified by gel permeation chromatography （GPC）. Identification and quantification were performed using gas chromatography-triple quadrupole fandem mass spectrometry （GC-MS-MS） in the selected reaction monitoring （SRM） mode. The efficiency of GPC was compared with that of solid phase extraction （SPE） for purifying crude extracts and the instrument parameters were optimized. The recovery rates of 16 PAH standards were in the range of 70.8%-123.1% from samples spiked with 4-6 μg/kg internal standard. The precision （RSD） of the developed method was 1.0%-6.5% with a limit of quantification of 0.22-0.74 μg/kg （r ≥ 0.9982）. Therefore, it is suitable for the analysis of 16 types of PAHs.

关 键 词：植物油 凝胶色谱净化 同位素稀释 气相色谱-串联质谱 多环芳烃 

分 类 号：TS207.3[轻工技术与工程—食品科学]