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郭萌萌, 吴海燕, 杨帆, 谭志军, 李兆新, 翟毓秀. 改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃[J]. 环境化学, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
引用本文: 郭萌萌, 吴海燕, 杨帆, 谭志军, 李兆新, 翟毓秀. 改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃[J]. 环境化学, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
shu
GUO Mengmeng, WU Haiyan, YANG Fan, TAN Zhijun, LI Zhaoxin, ZHAI Yuxiu. Determination of 16 polycyclic aromatic hydrocarbons in fishery products by improved QuEChERS-high performance liquid chromatography[J]. Environmental Chemistry, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
Citation: GUO Mengmeng, WU Haiyan, YANG Fan, TAN Zhijun, LI Zhaoxin, ZHAI Yuxiu. Determination of 16 polycyclic aromatic hydrocarbons in fishery products by improved QuEChERS-high performance liquid chromatography[J]. Environmental Chemistry, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
shu

改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃

  • 1.

    农业部水产品质量安全检测与评价重点实验室, 中国水产科学研究院黄海水产研究所, 青岛, 266071;

  • 2.

    国家水产品质量监督检验中心, 青岛, 266071;

  • 3.

    大连海洋大学, 大连, 116023

  • 基金项目:

    国家自然科学基金(41106109)

    中央级基本科研业务费项目(20603022012019, 20603022011004)资助.

Determination of 16 polycyclic aromatic hydrocarbons in fishery products by improved QuEChERS-high performance liquid chromatography

  • 1.

    Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture, China; Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao, 266071, China;

  • 2.

    National Center for Quality Supervision and Test of Aquatic Products, Qingdao, 266071, China;

  • 3.

    Dalian Ocean University, Dalian, 116023, China

  • Fund Project:

  • 摘要: 采用改进的QuEChERS,对水产样品进行提取、净化,用高效液相色谱仪-荧光/紫外检测器串联检测,建立了同时测定水产品中16种多环芳烃的高效液相色谱分析方法.样品经乙腈提取,Florisil+C18小柱净化,Waters PAH色谱柱分离,以乙腈-水为流动相进行梯度洗脱,外标法定量.本方法中,16种多环芳烃在各自相应浓度范围内线性关系良好,相关系数不低于0.999,检出限为0.1-3.6 μg·kg-1.采用该方法在鲤鱼、对虾和牡蛎中进行加标回收实验,回收率在75.0%-118.2%范围内,相对标准偏差(RSD)为2.6%-13.7%.应用本方法对环渤海湾的水产样品进行了调查分析,发现部分样品中含有PAHs,含量为2.11-147 μg·kg-1,为下一步开展相关风险评估工作打下了良好工作基础.
    Abstract: A method was developed for the simultaneous determination of 16 polycyclic aromatic hydrocarbons(PAHs)in fishery products by improved QuEChERS and high performance liquid chromatography with fluorescence and ultraviolet detection. After extraction with acetonitrile, the extract was purified by a Florisil+C18 column, then separated by HPLC on Waters PAH column (4.6 mm×250 mm,5 μm) by gradient elution using a mixture of acetonitrile and water as mobile phase. The external standard method was used to determine the content of 16 PAHs. The calibration curves were linear with correlation coefficients over 0.999. The limits of detection ranged from 0.1 μg·kg-1 to 3.6 μg·kg-1. The average spiked recoveries for 16 PAHs were between 75.0% and 118.2%, with relative standard derivations(RSDs)from 2.6% to 13.7%. The PAHs in some fishery products from circum-bohai sea region were found to be present at levels ranging from 2.11 μg·kg-1 to 147 μg·kg-1.
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  • 收稿日期:  2012-10-12
郭萌萌, 吴海燕, 杨帆, 谭志军, 李兆新, 翟毓秀. 改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃[J]. 环境化学, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
引用本文: 郭萌萌, 吴海燕, 杨帆, 谭志军, 李兆新, 翟毓秀. 改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃[J]. 环境化学, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
shu
GUO Mengmeng, WU Haiyan, YANG Fan, TAN Zhijun, LI Zhaoxin, ZHAI Yuxiu. Determination of 16 polycyclic aromatic hydrocarbons in fishery products by improved QuEChERS-high performance liquid chromatography[J]. Environmental Chemistry, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
Citation: GUO Mengmeng, WU Haiyan, YANG Fan, TAN Zhijun, LI Zhaoxin, ZHAI Yuxiu. Determination of 16 polycyclic aromatic hydrocarbons in fishery products by improved QuEChERS-high performance liquid chromatography[J]. Environmental Chemistry, 2013, 32(6): 1025-1031. doi: 10.7524/j.issn.0254-6108.2013.06.016
shu

改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃

  • 1.  农业部水产品质量安全检测与评价重点实验室, 中国水产科学研究院黄海水产研究所, 青岛, 266071;
  • 2.  国家水产品质量监督检验中心, 青岛, 266071;
  • 3.  大连海洋大学, 大连, 116023
  • 收稿日期:  2012-10-12
基金项目:

国家自然科学基金(41106109)

中央级基本科研业务费项目(20603022012019, 20603022011004)资助.

摘要: 采用改进的QuEChERS,对水产样品进行提取、净化,用高效液相色谱仪-荧光/紫外检测器串联检测,建立了同时测定水产品中16种多环芳烃的高效液相色谱分析方法.样品经乙腈提取,Florisil+C18小柱净化,Waters PAH色谱柱分离,以乙腈-水为流动相进行梯度洗脱,外标法定量.本方法中,16种多环芳烃在各自相应浓度范围内线性关系良好,相关系数不低于0.999,检出限为0.1-3.6 μg·kg-1.采用该方法在鲤鱼、对虾和牡蛎中进行加标回收实验,回收率在75.0%-118.2%范围内,相对标准偏差(RSD)为2.6%-13.7%.应用本方法对环渤海湾的水产样品进行了调查分析,发现部分样品中含有PAHs,含量为2.11-147 μg·kg-1,为下一步开展相关风险评估工作打下了良好工作基础.

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