加速溶剂提取凝胶渗透色谱净化气相色谱质谱快速测定玉米中多环芳烃  

Determination of Polycyclic Aromatic Hydrocarbons in Corn Using Accelerated Solvent Extraction and Gel Permeation Chromatography with Gas Chromatography-Mass Spectrometry

作　　者：佟玲[1] 周瑞泽[1] 吴淑琪[1] 张玲金[1] 

机构地区：[1]国家地质实验测试中心,北京100037

出　　处：《分析化学》2009年第3期357-362,共6页Chinese Journal of Analytical Chemistry

基　　金：国家地质实验测试中心基本科研费项目(No.20067csJ08)资助

摘　　要：研究了玉米中16种多环芳烃的快速分析方法。采用加速溶剂萃取法(ASE)对玉米样品进行提取,提取溶剂为二氯甲烷,萃取池中依次加入3g中性氧化铝吸附剂和10g待测样品,提取的同时能够在线净化除去小分子杂质。收集的提取液进一步用凝胶渗透色谱(GPC)除去样品中大分子油脂和色素,流动相为二氯甲烷,流速为3mL/min,收集9～13min的流出液,提取液浓缩定容至1mL后用GC-SIM-MS进行分析。16种PAHs以及4种替代物在2个浓度水平添加时的平均添加回收率在55.7%～145.3%之间;RSD为1.4%～16.8%;方法检出限为0.005～0.120ng/g。本方法简便、快速、准确,净化效果较好,满足残留分析的要求,且能应用于其它谷物样品的日常分析。A rapid analytical method for the determination of 16 PAHs in corn was proposed. The samples were extracted by accelerated solvent extraction （ASE） using dichloromethane as the extraction solvent. The ASE cell was filled up with 3.0 g Al2O3-N sorbent and 10.0 g corn. After the extraction, some small molecule compounds can be eliminated by the sorbent. The gel permeation chromatography（GPC） was used to remove the grease and pigment in the sample extract, and dichloromethane was used as mobile phase at a flow rate of 3.0 mL/min, the elution fractions was collected from 9 to 10 min. 1 mL concentrated solution was analyzed by GC-SIM-MS. The average recoveries of 16 PAHs and 4 surrogates were 55.7% - 145.3% , spiked at two dif- ferent levels. The relative standard deviations （RSD） for all the compounds were 1.4% - 16.8%. The detection limit （LOD） of the method varied between 0. 005 and 0. 120 ng/g. This method was fast, simple. It can be applied in routine analysis for different grist.

关 键 词：多环芳烃 加速溶剂萃取 凝胶渗透色谱 气相色谱质谱 玉米 残留分析 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]