固相萃取-高效液相色谱法检测药渣中残留泰乐菌素  

Determination of tylosin residue in pharmaceutical waste using solid phase extraction-high performance liquid chromatography

作　　者：王艳[1] 常璇[1] 马玉龙[1,2] 孙瑞珠[1] 王敏[1] 

机构地区：[1]宁夏大学化学化工学院,银川750021 [2]宁夏天然药物工程技术研究中心,银川750021

出　　处：《药物分析杂志》2013年第3期470-473,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(No.21067009)资助

摘　　要：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-0.02mol·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 col- umn ,and then determined using C18 -reversed -phase column with external standard. The mobile phase was aceto- nitrile -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-1 exhibited 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 de- viations were 2.4% -4. 1%. The detection limit was 0.05 mg · L-1. Conclusion ：This method can be used utili- zation for the detection of tylosin residue in pharmaceutical waste and feed.

关 键 词：固相萃取 高效液相色谱 泰乐菌素残留 药渣 资源利用 

分 类 号：R917[医药卫生—药物分析学]