高效液相色谱串联质谱法同时测定海产品中双酚A及烷基酚残留
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国家质检总局项目(2012IK173)


Simultaneously determining alkylphenols and bisphenol A residues in seafood by high-performance liquid chromatography with tandem mass spectrometry
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    摘要:

    建立了同时检测海产品中4种烷基酚包括4-壬基酚(4-NP)、4-辛基酚(4-OP)、4-n-壬基酚(4-n-NP)、4-t-辛基酚(4-t-OP)及双酚A(BPA)2类药物的高效液相色谱串联质谱的分析方法。样品经过乙腈超声提取和PSA固相萃取小柱净化后,使用高效液相色谱串联质谱仪测定,外标法定量。方法的检出限(信噪比S/N=3)及定量限(信噪比S/N=10)分别为0.07~0.30 μg/kg和0.2~1.0 μg/kg,4种烷基酚及双酚A在0.5~300.0 μg/L范围内线性关系良好,相关系数为0.991 8~0.999 9,在5~100 μg/kg范围内回收率试验通过空白样品加标来实现,平均加标回收率为60%~127%(n=6),相对标准偏差为2.2%~39.9%,该方法可满足进出口海产品中多种烷基酚及双酚A残留的检测需要。

    Abstract:

    A liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneously determining residues of four alkylphenols (APs) and bisphenol A in fresh fishes,shellfishes,and shrimps.The samples were ultrasonically extracted with acetonitrile,and then purified by PSA solid-phase extraction cartridge.Limits of detection were between 0.07 μg/kg and 0.30 μg/kg,and the limits of quantification were between 0.2 μg/kg and 1.0 μg/kg.The acceptable linearity was between 0.5-300.0 μg/L,and the related correlation coefficients were between 0.991 8-0.999 9.Recovery studies were carried out on spiked samples with concentrations between 5-100 μg/kg,and the average recoveries were between 60%-127%(n=6) with CVs of 2.2%-39.9%.The method was reliable,convenient and suitable for determining APs and BPA in seafood in import-export trade.

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俞雪钧,谷云云,冯睿,葛晓鸣,陈孟裕,倪梅林,胡霞林,钟莺莺.高效液相色谱串联质谱法同时测定海产品中双酚A及烷基酚残留[J].华中农业大学学报,2014,33(03):52-59

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  • 收稿日期:2013-11-29
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