凝胶渗透色谱-固相萃取-气相色谱-质谱法测定水产品中辛基酚、壬基酚和双酚A

doi:10.7506/spkx1002-6630-201324024

食品科学

凝胶渗透色谱-固相萃取-气相色谱-质谱法测定水产品中辛基酚、壬基酚和双酚A

黄会，邓旭修，张华威，刘云，徐英江，宫向红，张秀珍

1.上海海洋大学食品学院，上海 201306；2.山东省海洋水产研究所，山东烟台 264006；
3.山东省渔业环境监测站，山东烟台 264006；4.山东省海洋生态修复重点实验室，山东烟台 264006

出版日期:2013-12-25 发布日期:2014-01-03

Determination of Octylphenol, Nonylphenol and Bisphenol A in Aquatic Products by Gel Permeation Chromatography Coupled with Solid Phase Extraction and Gas Chromatography-Mass Spectrometry

HUANG Hui，DENG Xu-xiu，ZHANG Hua-wei，LIU Yun，XU Ying-jiang，GONG Xiang-hong，ZHANG Xiu-zhen

1. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China；2. Marine Fisheries Research Institute of Shandong Province, Yantai 264006, China；3. Shandong Fishery Environmental Monitoring Station, Yantai 264006,China；4. Shandong Provincial Key Laboratory of Restoration for Marine Ecology, Yantai 264006, China

Online:2013-12-25 Published:2014-01-03

摘要/Abstract

摘要：

对水产品中辛基酚(OP)、壬基酚(NP)和双酚A(BPA)测定的前处理方法进行优化，建立凝胶渗透色谱-固相萃取-气相色谱-质谱分析(GPC-SPE-GC-MS)方法。样品经乙酸乙酯超声提取，凝胶渗透-HLB固相萃取净化，七氟丁酸酐衍生化，进行GC-MS分析检测。结果表明：OP、NP、BPA在HP-5MS柱上有良好分离，方法检出限分别为0.2、0.1、0.1μg/kg，平均回收率OP不低于83.4%，NP不低于80.5%，BPA不低于81.3%，相对标准偏差范围为3.73%～9.19%。该方法应用于莱州湾部分水产品样品分析检测，简单便捷、灵敏度高，适用于水产品中OP、NP和BPA的检测。

关键词: 辛基酚, 壬基酚, 双酚A, 气相色谱-质谱, 凝胶渗透过滤-固相萃取, 水产品

Abstract:

On the basis of optimized sample pretreatment conditions, a method for the determination of octylphenol (OP),
nonylphenol (NP) and bisphenol A (BPA) in aquatic products has been developed by gel permeation chromatography
(GPC) coupled with solid phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS). The analytes were
extracted with ethyl acetate and purified seuquentially by gel permeation chromatography and HLB solid phase extraction
cartridges. After derivatization with heptafluorobutyrican anhydride (HFBA), the derivatives were determined by GCMS.
The results showed that the derivatives of the analytes were well separated by an HP-5MS column, and the limits of
detection for OP, NP and BPA were 0.2, 0.1 μg/kg and 0.1 μg/kg, respectively. The average recovery rates were more than
83.4%, 80.5% and 81.3%, respectively, with relative standard deviation (RSD) ranging from 3.73% to 9.19%. The method
has been used to determine seafood samples from Laizhou Bay with high sensitivity and reliability.

Key words: octylphenol, nonylphenol, bisphenol A, gas chromatography-mass spectrometry (GC-MS), gel permeation chromatography (GPC), solid phase extraction (SPE), aquatic product

黄会，邓旭修，张华威，刘云，徐英江，宫向红，张秀珍. 凝胶渗透色谱-固相萃取-气相色谱-质谱法测定水产品中辛基酚、壬基酚和双酚A[J]. 食品科学, doi: 10.7506/spkx1002-6630-201324024.

HUANG Hui，DENG Xu-xiu，ZHANG Hua-wei，LIU Yun，XU Ying-jiang，GONG Xiang-hong，ZHANG Xiu-zhen. Determination of Octylphenol, Nonylphenol and Bisphenol A in Aquatic Products by Gel Permeation Chromatography Coupled with Solid Phase Extraction and Gas Chromatography-Mass Spectrometry[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201324024.

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凝胶渗透色谱-固相萃取-气相色谱-质谱法测定水产品中辛基酚、壬基酚和双酚A

Determination of Octylphenol, Nonylphenol and Bisphenol A in Aquatic Products by Gel Permeation Chromatography Coupled with Solid Phase Extraction and Gas Chromatography-Mass Spectrometry

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