猪组织中替米考星残留的高效液相色谱检测方法研究

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

用乙腈和磷酸二氢钾缓冲液提取猪组织中替米考星,固相萃取柱净化,甲醇-乙腈-乙酸铵洗脱,紫外检测器290 nm处检测,建立了猪组织中替米考星残留的高效液相色谱检测方法.该方法检测肌肉、肝脏中替米考星的检测限分别为0.01和0.025 μg/g;定量限分别为0.02和0.05 μg/g.肌肉在0.02～2.0 μg/g添加范围内,平均回收率在84.2%～96.6%之间,变异系数在5.0%～8.2%之间;肝脏在0.05～5.0μg/g添加范围内,平均回收率在82.0%～92.8%之间,变异系数在5.8%～11.3%之间.本方法检测限低,分析简便、准确,符合残留分析的要求.

The Concentrations of tilmicosin residues in swine tissues were determined by HPLC. Swine tissues were extracted with acetonitrile and potassium dihydrogen phosphate buffer. The extracts were eluted by the C18 solid-phase extraction （SPE） cartridge. The residues were eluted from SPE cartridge with methanol-acetonitrile-ammonium acetate solution, and the eluate was determined by HPLC at 290 nm. The limits of quantitation （LOQ） were 0.02 μg/g and 0.05 μg/g for tilmicosin in muscle and liver, respectively. The limits of detection （LOD） were 0.01 μg/g and 0.025 μg/g for tilmicosin in muscle and liver, respectively. Recoveries of tilmicosin in muscle fortified at 0.02～2.0 μg/g and in liver fortified at 0.05～5.0 μg/g were in the range of 84.2%～96.6% and 82.0%～92.8%, respectively. Coefficients of variation were in the range of 5.0%～8.2% and 5.8%～11.3%, respectively. The method can meet the requirement for tilmicosin residue analysis.