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.pdf

1162013,Wo.34Mo.24
品学
※分析检
凝胶滲透色谱-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12,邓旭修,张华威,刘云,徐英江2,宫向红23,张秀珍24
(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264000
摘要:对水产品中辛基酚(OP)、王基酚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,凝胶滲透-HIB固相萃取净化,七氟丁了酸酐
行生化,进行GCMS分析检测。结果表明:OP、NP、BPA在HP-S5MS柱上有良好分离,方法检出限分别为02、01、
0.1pgkg,平均回收率OP不低于83.4%,NP不低于80.5%,BPA不低于813%,相对标准偏差范围为3.739%~9,19%。该
方法应用于菜州湾部分水产品样品分析检测,简单使捷、灵敏度高,适用于水产品中OP、NP和BPA的检测
关键同: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
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 2, DENG Xu-xi
ZHANG Hua-wei, LIU Yun", X0 Ying-jiang
2, GONG Xiang-hong, ZHANG Xiu-zhen2 3**
(1. College of Food Science and Techmology, Shanghai Ocean University, Shanghai 201306, China; 2. Marine Fisheries Research
Institute of Shandong Province, Yantai 264, hina 3. Shandong Fiey nvinmental Monitorin Station, Yantai 264006
China; 4. Shandong Provincial Key Laboratory of Restoration for Marine Ecology, Yantai 264005, China)
Abstract: On the basis of optimized sample ream ond, a met for the e mna on of octylphenol(P),
nonyl phenol (NP) and bisphenol A (BPA) in aquatic products has been developed by gel permeation chromatograph
( GPC)coupled with solid phase extraction(PE)and gas chromato rapy-mass spectromety(gc-ms). The analytes were
extracted with ethyl acetate and purified sequentially by gel permeation chmmato raphy and HLB solid phase extraction
cartridges. After derivatization with ep afluorobutyrican anhydride( HRB A) the derivatives were determined by GC
MS. 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, .I g/kg and D1 ug/kg, respectively. The average recover rates were more than
83.4, 80.5 and 81 3, eecel w lai sna e RD)rann fm.% 9. 1% Th me ho
has been used to determine seafood samples from Laizhou Bay with high sensitivity and reliabilit
Key words: octylphenol; nonylphenol; bisphenol A; gas chromatography-mass spectrometry(gc-ms); gel
permeation chromatography(GPC); solid phase extraction(PE); aquatic product
中图分类号:O67.71
文献标志码:A
文章编号:1002-6630(2013)24-0115-05
doi:10.7506/spkx1002-6630-201324024
辛基酚( octylphenol,OP)、王基酚( nonylphenol,NP)被排除或降解,最终都将进入海洋,污染海洋水体和水
和双酚A( bisphenol A,BPA)是常见内分泌干扰物",具产品-。在海洋环境?、水产品劉中已有检出,表明水
有和天然雌激素相似的结构和类睢激素活性,因而被称产品质量安全已受到威胁。
为酚类环境雌激素。这类物质理化性质稳定、可经由食
目前应用于OP、NP和BPA的分析方法主要是高
物链进行传递和浓缩、易于被动物体吸收和富集、难以效液相色谱( thigh performance liquid chromatography,
收稿日期:2013-01-28
基金项日:国家海洋公益性行业科研专项(201105013);山东省水生动物营养与侗料泰山学者岗位资助项日(2007~2012)
山东省科学技术发展计划项目(2012GHY11517):烟台市科技发展计划项目(2012134
作者简介:黄会(1985-),女,硕士研究生,研究方向为食品科学与工程。E-mail:hk57319@126.com
通信作者:张秀珍(1964-),女,研究员,木科,研究方向为食品质量安全与标准化。E-mail:zx7z0535501@126.com
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