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作 者:柯常亮[1] 刘奇[1] 王许诺[1] 陈洁文[1] 王增焕[1] 林颂雄[1] 蔡楠[1] 黄珂[1] 程波[2] 李刘冬[1]
机构地区:[1]中国水产科学研究院南海水产研究所,农业部水产品加工重点实验室,农业部水产品贮藏保鲜质量安全风险评估实验室(广州),广东广州510300 [2]中国水产科学研究院,北京100141
出 处:《食品与发酵工业》2015年第7期155-159,共5页Food and Fermentation Industries
基 金:国家农产品质量安全风险评估重大专项(项目编号:GJFP2014009);中央级公益性科研院所基本科研业务费专项(中国水产科学研究院南海水产研究所)(项目编号:2014TS10和2012TS15);中央级公益性科研院所基本科研业务费专项(中国水产科学研究院)(项目编号:2014C005)
摘 要:建立了气相色谱法同时测定水产品中28种多氯联苯同系物的分析方法。该方法用正己烷和二氯甲烷混合溶液超声辅助提取,提取液依次用浓H2SO4、中性Al2O3和弗罗里硅土净化,气相色谱定量,气相色谱串联质谱确证。结果显示,在2.00~200μg/L浓度范围内,28种多氯联苯同系物线性良好,相关系数r〉0.9991;加标量为0.5μg/kg和10.0μg/kg时,加标回收率范围分别为82.4%-106%和88.2%~97.8%,相对标准偏差范围分别为0.34%~5.95%和5.97%~13.3%;方法检测限和定量限范围分别为0.021~0.12μg/kg和0.07~0.40μg/kg。该方法适合批量水产品中28种多氯联苯同系物的同时测定。A method was established for simultaneous determination of 28 polychlorinated biphenyls (PCBs) in aquatic products using gas chromatography. Samples were extracted by the solution mixed with hexane and dichlo-romethane at the ratio of 1: 1. The extraction solution was purified with concentrated sulfuric acid, neutral aluminum and florisl and detected by gas chromatography. The analysis was then confirmed by gas chromatography coupled to tandem mass spectrometry. The results showed that the linear range was from 2.00 to 200 μg/L with good linearity (r 〉 0. 999 1 ). While spiked at 0.50 μg/kg and 10.0μg/kg, the recoveries of 28 PCBs ranged from 82.4% to 106% and 88.2% to 97.8%, respectively. The relative standard deviations (RSD) of the two spiked levels were ranged from 0.34% to 5.95% and 5.97% to 13.3% , respectively. Limit of detection (LOD) and Limit of quantification (LOQ) values were ranged from 0. 021 to 0. 12 μg/kgand 0.07 to 0.40 μg/kg, respectively. The method can be used to detect 28 PCBs in aquatic products simultaneously.
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