超高效液相色谱-串联质谱法测定配合饲料中大环内酯类药物

Analysis of macrolides in complete feeds by ultra-performance liquid chromatography-tandem mass spectrometry

试验建立配合饲料中大环内酯类药物(红霉素、罗红霉素、竹桃霉素、泰乐菌素、替米考星、交沙霉素)的超高效液相色谱-串联质谱检测方法。试验所用样品经用乙腈提取,磷酸盐缓冲液稀释,HLB固相萃取柱净化,BEH C18 column(2.1 mm×50 mm,1.7μm)色谱柱分离,0.1%甲酸水-乙腈梯度洗脱,电喷雾离子源正离子模式分析,外标法定量。结果显示,配合饲料中大环内酯类药物在10~100μg/kg添加水平下的回收率为72.7%~95.0%,RSD为1.3%~9.5%,方法的定量限为10μg/kg。研究表明,试验样品前处理过程简单、准确度及灵敏度较高,适用于配合饲料中大环内酯类药物的检测。

The experiment established a high performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS)was developed for the simultaneous determination of six macrolides(erythromycin,roxithromycin,oleandomycin,tylosin,tilmicosin and josamycin)in complete feeds.The samples were extracted with acetonitrile solution,diluted with phosphate buffer,followed by HLB solid phase extraction for further purification.The analytes were separated on an BEH C18 column(2.1 mm×50 mm,1.7μm)by gradient elution using 0.1%formic acid solution and acetonitrile as mobile phases,then analyzed by MS/MS with electrospray ionization in positive mode and quantified by external standard method.The results showed that at the level of 10~100μg/kg,the average recoveries for target compounds ranged from 72.7%~95.0%with relative standard deviations of 1.3%~9.5%.The limit of quantification of the method was 10μg/kg.The experiment indicates that the developed method is simple,accurate and sensitive,and it is suitable for the detection of macrolides in compound feeds.