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渔业研究 ›› 2022, Vol. 44 ›› Issue (1): 60-68.DOI: 10.14012/j.cnki.fjsc.2022.01.007

• 论文与报告 • 上一篇    下一篇

高效液相色谱-串联质谱法测定水产品中硝基咪唑类药物残留量

汤水粉,钱卓真,位绍红,王丽娟   

  1. 福建省水产研究所,福建 厦门 361013
  • 收稿日期:2021-09-26 修回日期:2021-10-18 出版日期:2022-02-25 发布日期:2022-02-17
  • 通讯作者: 汤水粉
  • 作者简介:汤水粉(1985-)女,硕士,工程师,主要从事水产品中药物残留的分析. E-mail:powder2005@126.com
  • 基金资助:
    福建省自然科学基金,福建省海洋与渔业结构调整专项;福建省海洋与渔业结构调整专项(2021HYJG02)

Determination of nitroimidazole drug residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS)

Shui-Fen TANG1, 1,shaohong WEI2,   

  • Received:2021-09-26 Revised:2021-10-18 Online:2022-02-25 Published:2022-02-17

摘要: 为建立高效液相色谱-串联质谱测定水产品中10种硝基咪唑类药物残留量的检测方法,样品经乙酸乙酯提取、正己烷除脂净化,采用高效液相色谱-串联质谱法在正离子模式下进行检测,外标法定量。结果表明,在优化的前处理方法和仪器条件下,10种硝基咪唑类药物在5.00~200 ng/mL的浓度范围内具有良好的线性关系,线性相关系数均大于0.995 0;在不同水产样品中分别添加1.00、2.00和5.00 μg/kg三个浓度水平时,加标回收率在70.2%~119%之间,相对标准偏差为1.46%~13.5%。该方法准确度和精密度均满足兽药残留检测的要求,而且操作简单、快速,可适用于水产品中硝基咪唑类药物的大批量样品检测。

关键词: 硝基咪唑, 水产品, 高效液相色谱-串联质谱

Abstract: A highly sensitive detection of 10 nitroimidazole drug residues in aquatic products has been achieved by optimizing the sample pretreatment methods combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS). The nitroimidazole drug residues in samples were extracted with ethyl acetate and removed fat by n-hexane, then quantified by the external standard method after detected in the positive ion mode by high performance liquid chromatography-tandem mass spectrometry. Under the optimized pretreatment methods and instrument conditions, the calibration curves were linear in a concentrations range of 5.00~200 μg/mL with R> 0.995 0. The average recovery was 70.2%~119% and the relative standard deviation was in the range of 1.46%~13.5% for spiked aquatic sample with 1.00 μg/kg,2.00 μg/kg and 5.00 μg/kg of nitroimidazoles. The accuracy and precision of the method was in accordance with the requirements of veterinary drug residue detection, and the operation was simple and fast. It showed that the method was suitable for the nitroimidazole drug residues detection of large quantities of samples.

Key words: nitroimidazole, aquatic products, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS)

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