UPLC-MS/MS法对动物源性食品中12种大环内酯类抗生素残留的测定

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法测定动物源性食品中12种大环内酯类抗生素(林可霉素、阿奇霉素、螺旋霉素、替米考星、竹桃霉素、红霉素、泰乐霉素、吉他霉素、罗红霉素、克拉霉素、麦迪霉素、交沙霉素)的方法.样品均质后,用乙腈提取,正己烷净化,无水硫酸钠脱水.乙腈提取液减压浓缩后,氮气流吹干,甲醇溶解定容;采用UPLC-MS/MS电喷雾多反应监测模式检测,基质匹配标准曲线定量.实验结果表明,12种大环内酯化合物在5 ～100 μg/kg范围内线性关系良好,检出限均为5.0 μg/kg,定量下限为10 μg/kg.5种空白基质样品中,10、25、50 μg/kg加标水平的平均回收率为60% ～117%,相对标准偏差均在20%以内.该方法灵敏度高、重复性好,各项技术指标均满足国内外相关法规要求,可用于动物源性食品中12种大环内酯类抗生素残留的检测.

Determination of 12 Macrolide Antibiotics Residues in Products of Animal Origin by Ultra Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for simultaneous determination of 12 macrolide antibiotics,e.g.lincomycin(LIN),azithromycin(AZI),spiramycin(SPM),tilmicosin(TIL),oleandomycin(OLD),josamycin(JOS),tylosin(TYL),kitasamycin(KIT),roxithromycin(ROM),clarithromycin(CLA),mydecamycin(MYD),erythromycin(ERM) in products of animal origin.Homogenized samples were extracted twice with acetonitrile.The extracts were partitioned with hexane to remove the animal fats and dehydrated with sodium sulphate anhydrous.The extract layer was evaporated to dryness and the residue was redissolved in methanol.Identification of 12 macrolide antibiotic was achieved by electrospray ionization tandem mass spectrometry in positive mode using multiple reaction monitoring(MRM) and quantification analysis was performed with matrix-matched standard calibration.The results indicated that,under the optimal conditions,the calibration curves showed good linearity for 12 macrolide antibiotics over the concentration range of 5-100 μg/kg.Detection limits were 5.0 μg/kg and quantification limits were 10 μg/kg for all the analytes.The mean recoveries varied from 60% to 117% at three spiked levels of 10,25,50 μg/kg.The RSDs were less than 20%.This method is sensitive and reproducible,and it meets the requirements of the domestic and international legislation.Therefore,it is suitable for the routinely determination of 12 macrolide antibiotics residues in products of animal origin.