猪排泄物中替米考星的高效液相色谱检测方法

 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。

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

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.