超高效液相色谱-串联质谱法同时测定饲料中6种大环内酯及林可胺类抗生素残留

Simultaneous Determination of Resides of Macrolide and Lincosamide in Animal Feed by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry

本研究建立UPLC-MSMS法同时测定饲料中泰乐菌素、吉他霉素、交沙霉素、螺旋霉素、林可霉素和克林霉素6种大环内酯及林可胺类抗生素残留量。样品处理采用乙腈提取,正己烷去除脂肪净化。分析采用XRODSⅡ色谱柱;流动相为0.1%(v/v)甲酸-水/0.1%(v/v)甲酸-乙腈溶液,梯度洗脱;正离子多反应监测模式;内标法进行定量。泰乐菌素、吉他霉素和林可霉素的检出限为20.0μg/kg,定量限为100.0μg/kg,线性范围均为50.0~500.0μg/L;交沙霉素、螺旋霉素和克林霉素的检出限均为1.0μg/kg,定量限为10.0μg/kg,线性范围为5.0~200.0μg/L。该方法专属性强、灵敏度高,分离度好,适用于饲料中6种大环内酯及林可胺类抗生素残留量的测定。

This is to set up a method to determine resides of 6 macrolide and lincosamide antibiotics in animal feed by ultra-performance liquid chromatography-tandem mass speftometry. After the samples were extracted by acetonitrile and removed fat and other impurities by hexane, XR-ODSⅡchromatographic column with 0.1%（v/v） formic acid water/0.1%（v/v） formic acid acetonitrile as mobile phase, liquid chromatography was separated by gradient elution, with positive ion multiple reaction monitoring and internal standard quantitative method. The detection limit of tylosin, kitasamycin and lincomycin was 20.0 μg/kg, the limit of quantitation was 100.0 μg/kg and the linear range was 50.0～500.0 μg/L. The detection limit of josamycin, spiramycin and clindamycin was1.0 μg/kg, the limit of quantitation was 10.0 μg/kg and the linear range was 5.0～200.0 μg/L.This method is highly specific, sensitive and separative, applicable to the determination of the resides of tylosin, kitasamycin, lincomycin, josamycin, spiramycin and clindamycin in animal feed.