中国农业科学 ›› 2005, Vol. 38 ›› Issue (12): 2531-2535 .

• 畜牧·兽医·资源昆虫 • 上一篇    下一篇

猪排泄物中替米考星的高效液相色谱检测方法

李存,沈建忠   

  1. 中国农业大学动物医学院
  • 收稿日期:2004-08-30 修回日期:1900-01-01 出版日期:2005-12-10 发布日期:2005-12-10
  • 通讯作者: 沈建忠

Determination of Tilmicosin Residues in Swine Excreta by High Performance Liquid Chromatography

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  1. 中国农业大学动物医学院
  • Received:2004-08-30 Revised:1900-01-01 Online:2005-12-10 Published:2005-12-10

摘要: 猪排泄物用乙腈和磷酸二氢钾缓冲液提取,C18 SPE柱净化,甲醇-乙腈-乙酸铵溶液洗脱,紫外检测器290 nm处检测,成功建立了猪排泄物中替米考星残留的高效液相色谱检测方法。该方法检测尿液、粪便中替米考星的定量限分别为0.025 ?g·ml-1和0.05 ?g·g-1,检测限分别为0.0125 ?g·ml-1和0.025 ?g·g-1。尿液在0.025 ?g·ml-1~2.0 ?g·ml-1添加范围内,回收率在83.4%~95.7%之间,日内变异系数在6.6%~8.9%之间,日间变异系数在6.4%~9.3%之间;粪便在0.05 ?g·g-1~5.0 ?g·g-1添加范围内,回收率在58.8%~73.9%之间,日内变异系数在8.7%~12.4%之间,日间变异系数在9.4%~16.5%之间。本方法检测限低,分析简便、准确,符合相关研究的要求。

关键词: 替米考星, 猪排泄物, 高效液相色谱, 残留检测

Abstract: The concentrations of tilmicosin residues in swine excreta were determined by HPLC. Swine excreta were extracted with acetonitrile and 0.1mol·L-1 potassium dihydrogen phosphate buffer (pH 2.5). The extracts were applied to C18 solid-phase extraction (SPE) cartridge. The residue was eluted from SPE cartridge with methanol-acetonitrile-ammonium acetate (20:80:0.77, v:v:g), and the eluate was determined by HPLC at 290 nm. Recoveries of tilmicosin in urine fortified at 0.025?g·ml-1-2.0?g·m;-1 and in faeces fortified at 0.05?g·g-1-5.0?g·g-1 were in the range of 83.4%-95.7% and 58.8%-73.9%, respectively. Coefficients of variation were in the range of 6.6%-8.9% and 8.7%-12.4%, respectively. The limits of quantification (LOQ) were 0.025?g·ml-1 and 0.05?g·g-1 for tilmicosin in urine and faeces, respectively. The limits of detection (LOD) were 0.0125?g·ml-1 and 0.025?g·g-1 for tilmicosin in urine and faeces, respectively. The method complied with the requirement for tilmicosin correlative study.

Key words: Tilmicosin, Swine excreta, High performance liquid chromatography, Residue determination