加速溶剂萃取/凝胶渗透色谱净化/气相色谱-三重四极杆质谱测定水产品中的持久性有机污染物  

Determination of Persistent Organic Pollutants(POPs)in Aquatic Products by Accelerated Solvent Extraction/Gel Permeation Chromatography/Gas Chromatography-tandem Mass Spectrometry

作　　者：荣茂 余婷婷 靳海斌 李珉 江丰 朱晓玲 刘迪 张莉 RONG Mao;YU Ting-ting;JING Hai-bin;LI Min;JIANG Feng;ZHU Xiao-ling;LIU Di;ZHANG Li(Hubei Provincial Institute for Food Supervision,Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Wuhan 430000,China)

机构地区：[1]湖北省食品质量安全监督检验研究院,湖北省食品质量安全检测工程技术研究中心,湖北武汉430000

出　　处：《现代食品科技》2020年第4期304-315,共12页Modern Food Science and Technology

基　　金：国家重点研发计划项目(2018YFC1602302、2018YFC1602303);湖北省自然科学基金项目(2018CFB339),湖北省食品药品监督管理局科研项目(201602005)。

摘　　要：建立了一种加速溶剂萃取/凝胶渗透色谱净化/气相色谱三重四极杆质谱同时检测水产品中46种典型持久性有机污染物的方法。水产样品经-105℃、100 mbar条件下的冷冻干燥处理后,加入硅藻土混合碾磨均匀后,经加速溶剂萃取、凝胶渗透色谱净化,使用萘-d、芴-d、蒽-d、■-d作为内标,采用气相色谱三重四极杆质谱的多反应监测模式对水产品中的16种多环芳烃、30种有机氯农药进行定性定量分析。在100℃、1500 psi条件下以二氯甲烷:己烷(1:1,V/V)对46种有机污染物进行萃取,收集凝胶渗透色谱中7.5~16 min馏出液,浓缩定容上机分析。46种持久性有机污染物分离效果良好,相关系数R^2均在0.99以上,低(10μg/kg)、中(50μg/kg)、高(100μg/kg)3个水平的加标回收率均在81.0%~121.0%之间,相对标准偏差(RSD,n=6)在4.1%~11.0%之间,方法检出限为0.0185μg/kg^0.7377μg/kg(干重)。该方法采用加速溶剂萃取仪和凝胶渗透色谱仪进行前处理,可实现前处理无人值守,大大提升检验效率,且方法稳定性好,灵敏度和回收率高,是分析水产品中痕量持久性有机污染物的较好方法。An improved method based on accelerated solvent extraction/gel chromatography purification/gas chromatography-triplequadrupole mass spectrometry was set up to detect 46 POPs in aquatic products.The aquatic products were freeze-dried at-105℃and 100 mbar and then uniformly mixed with diatomaceous earth.The accelerated solvent extraction and gel chromatography purification were used to remove grease.The quantitation and qualification analysis of 16 kinds of polycyclic aromatic hydrocarbons and 30 kinds of organochlorines were performed by gas chromatography-triple-quadrupole mass spectrometry(GCMS/MS)in the multiple reaction monitoring(MRM)mode,using Naphthalene-d,Acenaphthene-d,Anthracene-d,Chrysene-d as internal standards.46 organic contaminants were extracted with dichloromethane:hexane(1:1,V/V)at 100℃and 1500 psi,and their distillate(7.5~16 min)was collected.The separation of 46 POPs was good,and the correlation coefficient R^2 was above 0.99.The recoveries of low(10μg/kg),medium(50μg/kg)and high(100μg/kg)levels were between 81.0%and 121.0%,the relative standard deviations(RSD,n=6)were between 4.1%and 11.0%,and the detection limit was 0.0185μg/kg^0.7377μg/kg(dry weight).This method,with accelerated solvent extraction and gel chromatography purification as pretreatments,has good stability,low detection limit,and a high recovery rate.It is a promising method for analyzing trace POPs in aquatic products.

关 键 词：水产品 持久性有机污染物 气相色谱-三重四极杆质谱 加速溶剂萃取 凝胶渗透色谱 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]