食品科学

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高效液相色谱法测定硝基呋喃类药物代谢物及其在对虾体内的代谢

辛少平1,2,邓建朝1,杨贤庆1,岑剑伟1,魏 涯1,郝淑贤1,李来好1,*   

  1. 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,
    国家水产品加工技术研发中心,广东 广州 510300;2.上海海洋大学食品学院,上海 201306
  • 出版日期:2014-12-25 发布日期:2014-12-29
  • 通讯作者: 李来好
  • 基金资助:

    “十二五”国家科技支撑计划项目(2012BAD28B00);国家现代农业(罗非鱼)产业技术体系建设专项(CARS-49);
    广东省水产品质量安全专项(2130109A-2-1);省部产学研结合示范基地项目(2011B090500015);
    广东省海洋渔业科技推广专项(B201300C03)

Determination of Nitrofuran Metabolites by High Performance Liquid Chromatography and Their Metabolism in Shrimp

XIN Shao-ping1,2, DENG Jian-chao1, YANG Xian-qing1, CEN Jian-wei1, WEI Ya1, HAO Shu-xian1, LI Lai-hao1,*   

  1. 1. National R&D Center for Aquatic Product Processing, Key Laboratory of Aquatic Product Processing, Ministry of Agriculture,
    South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou 510300, China;
    2. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China
  • Online:2014-12-25 Published:2014-12-29
  • Contact: LI Lai-hao

摘要:

建立高效液相色谱法测定对虾中胺基脲(semicarbazide,SEM)、1-氨基-2-内酰脲(1-aminohydantoin,AHD)、5-甲基吗啉-3-氨基-2-唑烷基酮(5-morpholinomethyl-3-amino-2-oxazolidone,AMOZ)和3-氨基-2-恶唑基酮(3-amino-2-oxazolidone,AOZ)4 种硝基呋喃类药物代谢物。采用含100 g/L三氯乙酸的甲醇-水(50∶50,V/V)溶液提取,邻氯苯甲醛衍生,经乙酸乙酯萃取、异辛烷净化,以0.05 mol/L乙酸铵-乙腈(30∶70,V/V)为流动相,反相高效液相色谱分析,外标法定量。结果表明,4 种待测物在0.1~50 nmol/mL 浓度范围内线性良好,检出限分别为SEM 0.75 μg/kg、AHD 1.2 μg/kg、AMOZ 2.0 μg/kg、AOZ 1.0 μg/kg。停药后4 种硝基呋喃类药物代谢物在对虾肌肉内富集最高含量分别为51.5、35.8、79.3 μg/kg和127 μg/kg,代谢物残留低于0.5 μg/kg所需代谢时间为SEM 21 d、AHD 15 d、AMOZ 17 d和AOZ 23 d。

关键词: 高效液相色谱, 硝基呋喃代谢产物, 代谢规律, 对虾

Abstract:

A high performance liquid chromatography (HPLC) method for the determination of nitrofuran metabolites
in shrimp has been established. After being extracted by 100 g/L trichloroacetic acid in methanol-water (50:50, V/V), the
four metabolites semicarbazide (SEM), 1-aminohydantoin (AHD), 5-morpholinomethyl-3-amino-2-oxazolidone (AMOZ) and
3-amino-2-oxazolidone (AOZ), were reacted with 2-chlorobenzaldehyde. The analytes were separated in a C18 column with
0.05 mol/L ammonium acetate-acetonitrile (30:70, V/V) as the mobile phase and detected by a UV detector. SEM, AHD, AMOZ
and AOZ were quantified by external standard method. The response signals were all linearly proportional to concentrations of
the four metabolites in the range of 0.1–50 nmol/mL, and the limits of detection (LODs) were calculated as 0.75, 1.2, 2.0 and
1.0 μg/kg, respectively. The maximum values of the four metabolites accumulated in shrimp muscle were found to be 51.5,
35.8, 79.3 and 127 μg/kg after the discontinuation of the drugs, and the elimination life turns out to be 21, 15, 17 and 23 days
in this study, respectively.

Key words: high performance liquid chromatography (HPLC), nitrofuran metabolites, metabolism, shrimp

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