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液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量

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邢丽红, 孙伟红, 彭吉星, 孙晓杰, 郑关超, 李兆新. 液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量[J]. 环境化学, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
引用本文: 邢丽红, 孙伟红, 彭吉星, 孙晓杰, 郑关超, 李兆新. 液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量[J]. 环境化学, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
shu
XING Lihong, SUN Weihong, PENG Jixing, SUN Xiaojie, ZHENG Guanchao, LI Zhaoxin. Determination of nitrofuran metabolites residues in shellfish tissues by high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
Citation: XING Lihong, SUN Weihong, PENG Jixing, SUN Xiaojie, ZHENG Guanchao, LI Zhaoxin. Determination of nitrofuran metabolites residues in shellfish tissues by high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
shu

液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量

  • 1.

    农业农村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.

    农业农村部水产品质量安全风险评估实验室(青岛), 青岛, 266071

  • 基金项目:

    国家自然科学基金（41806148），中国水产科学研究院黄海水产研究所基本科研业务费（20603022018016）和2018年国家水产品质量安全风险评估项目（GJFP201800901）资助

Determination of nitrofuran metabolites residues in shellfish tissues by high performance liquid chromatography-tandem mass spectrometry

  • 1.

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

  • 2.

    Laboratory of Quality & Safety Risk Assessment for Aquatic Products (Qingdao), Ministry of Agriculture and Rural Affairs, P.R.China, Qingdao, 266071, China

  • Fund Project: Supported by National Science Foundation of China (41806148), Central Public-interest Scientific Institution Basal Research Fund, YSFRI, CAFS(20603022018016) and 2018 National Risk Assessment Program of Aquatic Products for Quality and Safety(GJFP201800901)

  • 摘要: 建立了液相色谱-串联质谱法测定贝类产品中硝基呋喃类代谢物残留量的分析方法.贝类组织中残留的硝基呋喃类蛋白结合态代谢物在酸性条件下水解，用2-硝基苯甲醛衍生化，经乙酸乙酯液-液萃取、浓缩及基质分散固相萃取和超滤净化后，采用液相色谱串联质谱仪测定，以电喷雾离子源正离子扫描模式进行质谱分析，内标法定量.硝基呋喃类代谢物在0.5—20 μg·L-1范围内线性关系良好，相关系数R2>0.999.4种硝基呋喃类代谢物添加水平为1.00， 2.50、10.0 μg·kg-1时，平均回收率在90.1%—99.5%之间，批内和批间变异系数均-1.本方法灵敏、高效、简单、重现性好，满足贝类产品中硝基呋喃类代谢物残留量的检测要求.
    Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of nitrofuran metabolites residues in shellfish tissues. The residues of protein adducts from nitrofuran metabolites in shellfish tissues were hydrolyzed by HCl, followed by derivatizing with nitrobenzaldehyde. The resulting derivatives were extracted with ethyl acetate, and the organic layer was concentrated by a stream of nitrogen gas. After purification by matrix dispersed solid phase extraction combined with ultrafiltration, the samples were analyzed by LC-MS/MS using internal standard method. Electrospray ionization was applied and operated in positive ion mode. The calibration curve showed a good linearity in the range of 0.5-20 μg·L-1 with the correlation coefficient over 0.999. The average recoveries for the spiked samples at concentrations of 1.00, 2.50 and 10.0 μg·kg-1 ranged from 90.1% to 99.5% with intra and inter batch relative standard deviations below 15%. The limit of detection of nitrofuran metabolites was 0.50 μg·kg-1. This approach is proved to be a simple and efficient method to identify and quantify nitrofuran metabolites in shellfish tissues with satisfactory sensitivity and repeatability.
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  • 收稿日期:  2018-04-16
  • 刊出日期:  2019-02-15
邢丽红, 孙伟红, 彭吉星, 孙晓杰, 郑关超, 李兆新. 液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量[J]. 环境化学, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
引用本文: 邢丽红, 孙伟红, 彭吉星, 孙晓杰, 郑关超, 李兆新. 液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量[J]. 环境化学, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
shu
XING Lihong, SUN Weihong, PENG Jixing, SUN Xiaojie, ZHENG Guanchao, LI Zhaoxin. Determination of nitrofuran metabolites residues in shellfish tissues by high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
Citation: XING Lihong, SUN Weihong, PENG Jixing, SUN Xiaojie, ZHENG Guanchao, LI Zhaoxin. Determination of nitrofuran metabolites residues in shellfish tissues by high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2019, 38(2): 287-296. doi: 10.7524/j.issn.0254-6108.2018041601
shu

液相色谱-串联质谱法测定贝类组织中硝基呋喃类代谢物残留量

  • 1.  农业农村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.  农业农村部水产品质量安全风险评估实验室(青岛), 青岛, 266071
  • 收稿日期:  2018-04-16
基金项目:

国家自然科学基金（41806148），中国水产科学研究院黄海水产研究所基本科研业务费（20603022018016）和2018年国家水产品质量安全风险评估项目（GJFP201800901）资助

摘要: 建立了液相色谱-串联质谱法测定贝类产品中硝基呋喃类代谢物残留量的分析方法.贝类组织中残留的硝基呋喃类蛋白结合态代谢物在酸性条件下水解，用2-硝基苯甲醛衍生化，经乙酸乙酯液-液萃取、浓缩及基质分散固相萃取和超滤净化后，采用液相色谱串联质谱仪测定，以电喷雾离子源正离子扫描模式进行质谱分析，内标法定量.硝基呋喃类代谢物在0.5—20 μg·L-1范围内线性关系良好，相关系数R2>0.999.4种硝基呋喃类代谢物添加水平为1.00， 2.50、10.0 μg·kg-1时，平均回收率在90.1%—99.5%之间，批内和批间变异系数均-1.本方法灵敏、高效、简单、重现性好，满足贝类产品中硝基呋喃类代谢物残留量的检测要求.

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