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鲭鱼罐头中7种多氯联苯的测定——亚临界水萃取-气相色谱法
引用本文:王婷婷,;李莉,;陈易晖,;徐颖,;聂诚刚,;刘望才,;房江华,;高浩其.鲭鱼罐头中7种多氯联苯的测定——亚临界水萃取-气相色谱法[J].宁波工程学院学报,2014(2):1-6.
作者姓名:王婷婷  ;李莉  ;陈易晖  ;徐颖  ;聂诚刚  ;刘望才  ;房江华  ;高浩其
作者单位:[1]宁波工程学院,浙江宁波315016; [2]象山出入境检验检疫局,浙江象山310014; [3]北仑出入境检验检疫局,浙江北仑315800
基金项目:浙江省自然科学基金(项目编号LQ12B05001);宁波市自然科学基金(项目编号2012A610091);宁波市创新团队(2011B82002);北仑科技创新基金和2012校立项(项目编号46)。
摘    要:建立了同时检测鲭鱼罐头中7种多氯联苯(PCBs)的亚临界水萃取-气相色谱分析方法。亚临界水中加入活性炭纤维为固相萃取剂,在200℃的条件下,提取40 min,随后,用2 mL乙酸乙酯洗脱。结果表明,该方法测定PCBs含量的线性范围为0.001~0.100μg/mL;在2.0、10.0、50.0μg/kg(n=6)的添加水平下,回收率在79.4%~91.0%之间,测定结果的相对标准偏差(RSD)为3.1%~12.3%;检出限(S/N=3)为0.016~0.046μg/kg;定量限(S/N=10)为0.048~0.139μg/kg。该方法绿色环保、稳定、可靠,适用于鲭鱼罐头中多氯联苯的检测。

关 键 词:亚临界水萃取  气相色谱  多氯联苯  鲭鱼罐头

Determination of 7 Polyclalorinated Biophenyls in Canned Mackerel --Sub-critical Water Extraction-gas Chromatography Method
Affiliation:WANG Ting-ting, LI Li, HEN Yi-hui, XU Ying, NIE Cheng-gang, LIU Wang-cai, FANG Jiang-hua, GAO Hao-qi(1. Ningbo University of Technology, Ningbo, Zhejiang, 315016, China; 2. Xiangshan Entry-Exit Inspection and Quarantine Bureau, Xiangshan, Zhejiang, 310014, China; 3. Beilun Entry-Exit Inspection and Quarantine Bureau, Beilun, Zhejiang, 315800, China)
Abstract:A method for the simultaneous determination of 7 polychlorinated biophenyls (PCBs) in canned Mackerel by sub-critical water extraction coupled with gas chromatography is developed. PCBs are extracted by 200 ℃ sub-critical water for 40 min, and adsorbed on active carbon fibers at the same time. And then, PCBs are desorbed by 2 mL ethyl acetate. The results show that the linear range for the determination of PCBs in canned Mackerel is between 0.001~0.100 μg/mL with the limit of detection (LOD, S/N=3) of 0.016~0.046 μg/kg and the limit of quantification (LOQ, S/N=10) of 0.048~0.139 μg/kg. At the spiked level of 2.0、10.0、50.0 μg/kg (n=6), the recoveries range from 79.4% to 91.0% with the relative standard deviations (RSDs) between 3.1% and 12.3%. The developed method is environmentally-friendly and suitable for the simultaneous determination of 7 PCBs in canned Mackerel with high accuracy and high precision.
Keywords:Sub-critical water extraction  gas chromatography (GC)  polychlorinated biophenyls (PCBs)  canned Mackerel
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