湖北农业科学 ›› 2023, Vol. 62 ›› Issue (10): 172-177.doi: 10.14088/j.cnki.issn0439-8114.2023.10.030

• 检测分析 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定水产品中10种硝基咪唑类药物残留量

谢云波, 易鸣, 童文羽, 曾智, 朱志强, 石义付   

  1. 湖北省水产科学研究所,武汉 430071
  • 收稿日期:2022-07-06 发布日期:2023-11-14
  • 通讯作者: 石义付(1973-),男,湖北咸宁人,正高级工程师,硕士,主要从事水产品养殖环境研究,(电话)18162797399。
  • 作者简介:谢云波(1994-),男,湖北武汉人,本科,专业方向为水产品兽药残留及水产品养殖环境,(电话)15172424232(电子信箱)969769659@qq.com。

Simultaneous determination of 10 nitroimidazole drugs residues in aquatic products by high-performance liquid chromatography-tandem mass spectrometry

XIE Yun-bo, YI Ming, TONG Wen-yu, ZENG Zhi, ZHU Zhi-qiang, SHI Yi-fu   

  1. Hubei Institute of Fisheries Science Research, Wuhan 430071, China
  • Received:2022-07-06 Published:2023-11-14

摘要: 建立了水产品中10种硝基咪唑类药物残留量高效液相色谱法-串联质谱检测方法。样品经乙酸乙酯提取,减压蒸馏后,正己烷净化,再用10%甲醇溶解残渣,再通过C18色谱柱(150 mm×2 mm,5 μm)进行分离,0.20%甲酸水溶液-乙腈为流动相,梯度洗脱,采用高效液相色谱法-串联质谱法对目标化合物进行分析。方法检出限为0.04~0.30 μg/kg,定量限为0.50~1.00 μg/kg,在1~150 μg/L范围内线性关系良好,相关系数(R2)>0.998 00。在5.0、7.5、10.0、15.0、20.0 μg/kg的加标水平下,回收率为73.0%~116.2%,相对标准偏差(RSD)为0.43%~9.53%。该方法操作简便、灵敏度高、重现性好,适用于大批量样品的检测。

关键词: 水产品, 硝基咪唑类药物, 高效液相色谱-串联质谱法, 药物残留量

Abstract: A high-performance liquid chromatography-tandem mass spectrometry method was established for the detection of nitroimidazole drugs residues in aquatic products. The sample was extracted with ethyl acetate, distilled under reduced pressure, purified with n-hexane, and the residue was dissolved in 10% methanol before passing through a C18 chromatographic column (150 mm×2 mm, 5 μm). Separation was carried out using 0.20% formic acid aqueous solution acetonitrile as the mobile phase, gradient elution was performed, and the target compound was analyzed using high-performance liquid chromatography tandem mass spectrometry. The detection limit of the method was 0.04~0.30 μg/kg, the quantitative limit was 0.50~1.00 μg/kg, the linear relationship was good within the range of 1~150 μg/L, and the correlation coefficient (R2) was >0.998 00. At spiked level of 5.0, 7.5, 10.0, 15.0, and 20.0 μg/kg, the recovery rate was 73.0%~116.2%, and the relative standard deviation (RSD) was 0.43%~9.53%. This method was easy to operate, highly sensitive, and had good reproducibility, making it suitable for the detection of large batches of samples.

Key words: aquatic products, nitroimidazole drugs, high performance liquid chromatography tandem mass spectrometry, drugs residues

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