色谱

色谱

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高效液相色谱法测定猪组织中咪唑苯脲残留研究

于慧敏, 黄显会*, 钟家林, 杨刚, 方秋华   

  1. 华南农业大学国家兽药残留基准实验室, 广东 广州 510642
  • 收稿日期:2011-02-14 修回日期:2011-05-12 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 黄显会,高级兽医师.
  • 基金资助:

    2009年农业行业标准制定和修订计划项目

Determination of imidocarb residue in swine tissues by high performance liquid chromatography

  1. National Reference Laboratory of Veterinary Drug Residues (SCAU), South China Agricultural University, Guangzhou 510642, China
  • Received:2011-02-14 Revised:2011-05-12 Online:2011-08-28 Published:2011-09-28

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摘要： 建立了高效液相色谱(HPLC)测定猪可食性组织中咪唑苯脲残留的方法。猪组织经β-葡萄糖苷酶水解后,用1 mol/L盐酸提取,再用正己烷-异戊醇(3:2, v/v)混合溶剂萃取净化。以乙腈和0.0075 mol/L戊烷磺酸钠水溶液(含0.1%三乙胺,pH 3.0)作为流动相,经C18反相色谱柱分离后用紫外检测器检测。结果表明: 该方法在咪唑苯脲含量为10～10000 μg/L范围内呈现良好的线性关系,相关系数大于0.999;空白组织中加标样品的检出限(LOD)为10 μg/kg,定量限(LOQ)为20 μg/kg。在定量限、最高残留限量(MRL)、2倍MRL添加水平下,不同组织的平均回收率为80.04%～110.32%,相对标准偏差为0.82%～10.00%。表明该检测方法简单、灵敏,适用于猪组织中咪唑苯脲残留的定量检测。

关键词: 高效液相色谱法, 可食性组织, 咪唑苯脲, 兽药残留, 猪

Abstract: A quantitive method for the determination of imidocarb residue in edible tissues of swine by high performance liquid chromatography (HPLC) was developed. The analyte was digested by β-glucosidase first, and then extracted with 1 mol/L hydrochloric acid. The aqueous phase was back-extracted with the mixture of hexane-isoamyl alcohol (3:2, v/v) for the purification. The mobile phases were acetonitrile (phase A) and 0.0075 mol/L 1-pentansulfonic acid sodium aqueous solution containing 0.1% triethylamine, adjusted to pH 3.0 with glacial acetic acid (phase B). The analyte was detected by ultraviolet absorption spectroscopy after the separation was achieved on a C18 RP column. The linear range was 10~10000 μg/L, and the correlation coefficient was more than 0.999. The limit of detection (LOD) was 10 μg/kg, and the limit of qualification (LOQ) was 20 μg/kg. The mean recoveries of imidocarb in swine tissues at the added levels of LOQ, MRL (maximum residue limit) and 2MRL ranged from 80.04% to 110.32%, and the relative standard deviations (RSDs) of intra- and inter-day analyses ranged from 0.82% to 10.00%. The method is simple and sensitive for the quantification of imidocarb residue in swine tissues.

Key words: edible tissues, imidocarb, swine, veterinary drug residue, high performance liquid chromatography (HPLC)