固相萃取-高效液相色谱法检测药渣中残留泰乐菌素

目的:建立了药渣中残留泰乐菌素的固相萃取-高效液相色谱测定方法。 方法:药渣中残留泰乐菌素经甲醇提取,正己烷脱脂,C₁₈固相萃取柱净化,然后用Agilent HC-C₁₈ 反相色谱柱,紫外检测器,外标法定量检测。流动相为乙腈-0.02 mol·L^-1磷酸二氢钾溶液,等度洗脱,流速1 mL·min^-1。 结果:泰乐菌素含量在0.1~100 mg·L^-1的范围内呈良好线性关系,在16,20,24 mg·L^-1添加水平下的回收率为92.9%~107.1%,RSD为2.4%~4.1%,检出限为0.05 mg·L^-1。 结论:本法适用于药渣、饲料等样品中泰乐菌素残留量的测定。

Objective: To develop a method for the determination of tylosin residue in pharmaceutical waste using solid phase extraction (SPE)-high performance liquid chromatography with a UV detection system. Methods: Tylosin in pharmaceutical waste was extracted using methanol,defatted with hexane,purified on a C₁₈-SPE column,and then determined using C₁₈-reversed-phase column with external standard.The mobile phase was acetonitrile-0.02 mol·L^-1 phosphate buffer and the flow rate was 1.0 mL·min^-1 with isocratic elution. Results: The tylosin concentrations within the range of 0.1-100 mg·L^-1exhibited a better linearity.The recoveries at spiked concentration of 16,20,24 mg·L^-1 were in the range of 92.9%-107.1%, and the relative standard deviations were 2.4%-4.1%.The detection limit was 0.05 mg·L^-1. Conclusion: This method can be used utilization for the detection of tylosin residue in pharmaceutical waste and feed.