色谱

色谱 ›› 2017, Vol. 35 ›› Issue (9): 995-1002.DOI: 10.3724/SP.J.1123.2017.04033

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱法同时测定牛组织中三氮脒和氯化氮氨菲啶残留

周雨卉, 曾振灵, 余静贤, 刘戎, 潘丽花, 钟秋玉, 陈红   

  1. 华南农业大学兽医学院, 国家兽药残留基准实验室, 广东 广州 510642
  • 收稿日期:2017-04-27 出版日期:2017-09-08 发布日期:2017-09-15
  • 通讯作者: 陈红,Tel:(020)85283034,E-mail:shuyi@scau.edu.cn.
  • 基金资助:

    农业行业标准制定项目（农财发[2009]105号）.

Simultaneous determination of diminazene aceturate and isometamidium chloride residues in cattle tissues by high performance liquid chromatography with solid-phase extraction

ZHOU Yuhui, ZENG Zhenling, YU Jingxian, LIU Rong, PAN Lihua, ZHONG Qiuyu, CHEN Hong   

  1. College of Veterinary Medicine, South China Agricultural University, National Reference Laboratory of Veterinary Drug Residues, Guangzhou 510642, China
  • Received:2017-04-27 Online:2017-09-08 Published:2017-09-15
  • Supported by:

    Agricultural Industry Criteria Formulate Project (Agricultural Finance[2009] No. 105).

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摘要：

建立了固相萃取-高效液相色谱同时检测牛组织中三氮脒（DIM）和氯化氮氨菲啶（ISM）残留的分析方法。针对不同的组织样品采用不同比例的水-乙腈溶液提取药物，结合Oasis WCX固相萃取小柱净化富集。采用Spherisorb CN柱（250 mm×4.6 mm， 5 μm）对药物进行分离，以乙腈和0.05 mol/L甲酸铵溶液（pH 2.4）为流动相，梯度洗脱，紫外检测波长为380 nm。牛组织中DIM和ISM的检出限（S/N ≥ 3）为0.01 mg/kg，定量限（S/N ≥ 10）为0.025 mg/kg。牛组织中DIM和ISM在各自的线性范围内线性关系良好（r ≥ 0.9993）。DIM和ISM在低、中、高添加水平下的回收率为82.2%~97.6%，日内精密度和日间精密度分别为0.3%~5.2%（n=5）和1.3%~5.2%（n=15）。结果表明，建立的方法重复性好，灵敏度高，操作简便，适用于牛组织中DIM和ISM的残留检测。

关键词: 多残留检测, 高效液相色谱, 固相萃取, 氯化氮氨菲啶, 牛组织, 三氮脒

Abstract:

A method for the simultaneous determination of trypanocidal diminazene aceturate (DIM) and isometamidium chloride (ISM) that containing benzamidine groups in cattle tissues was developed by high performance liquid chromatography (HPLC) with solid-phase extraction (SPE). The tissue samples were extracted with different proportions of water-acetonitrile, then were cleaned up by Oasis WCX cartridges. DIM and ISM were separated by HPLC with a Spherisorb CN column (250 mm×4.6 mm, 5 μm). Acetonitrile-0.05 mol/L ammonium formate solution (pH 2.4) was used as mobile phases with gradient elution. The detection wavelength of UV was set at 380 nm. The limits of detection (LODs) and the limits of quantification (LOQs) of DIM and ISM in cattle tissues were 0.01 mg/kg and 0.025 mg/kg, respectively. The correlation coefficients (r) of DIM and ISM in cattle tissues were not less than 0.9993. The average recoveries of DIM and ISM at three spiked levels were 82.2%-97.6% with the intra-day relative standard derivations (RSDs) of 0.3%-5.2% (n=5) and inter-day RSDs of 1.3%-5.2% (n=15). The method was successfully applied to the analysis of DIM and ISM in cattle tissues. The method is rapid, sensitive and repeatable for the determination of diminazene aceturate and isometamidium chloride in cattle tissues.

Key words: cattle tissues, diminazene aceturate (DIM), high performance liquid chromatography (HPLC), isometamidium chloride (ISM), multi-residue determination, solid-phase extraction (SPE)

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