超高效液相色谱-串联质谱法测定猪组织中泰拉霉素及其代谢物残留量

Determination of Tulathromycin and Its Metabolite in Pig Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

对猪组织中泰拉霉素及其代谢物残留量的测定方法进行了研究,基于超高效液相色谱-串联质谱建立了猪肉、肝脏、肾脏中泰拉霉素及其代谢物残留量的测定方法。试样经乙腈-0.1%甲酸水(7+3)提取,MCX柱净化,氮吹后用乙腈-0.1%甲酸水(1+9)复溶,正离子扫描,多反应监测模式下上机分析,基质外标法定量。结果表明,泰拉霉素及其代谢物在5~500μg/kg的浓度范围内呈现良好的线性关系,相关系数(R2)均>0.99;该方法的检出限为5μg/kg(猪肉:2μg/kg),定量限为10μg/kg;在不同浓度添加水平下,平均回收率为72.6%~105.8%,日内相对标准偏差为0.5%~12.1%,日间相对标准偏差为2.9%~8.1%。该方法简便、快速、灵敏度高、重现性好,适用于猪组织中泰拉霉素及其代谢物残留量的测定。

A method for the determination of tulathromycin and its metabolite in pig tissues was developed by ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted by acetonitrile-0.1%formic acid aqueous(7+3)and cleaned by MCX solid phase extraction column,and the residue was redissolved with acetonitrile-0.1%formic acid aqueous(1+9)after the dried under a N2 atmosphere.In the positive ion mode and multi reaction monitoring mode,the analytes were quantified by matrix external standard.The results of tulathromycin and its metabolite were linear in the range of 5~500μg/kg with the correlation coefficients(R2)>0.99.The limits of detection(LODs)and the limits of quantification(LOQs)were 5μg/kg(2μg/kg for pork)and 10μg/kg,respectively.The average recoveries of tulathromycin and its metabolite under different spiked levels were 72.6%~105.8%with intraday relative standard deviations(RSDs)of 0.5%~12.1%and interday relative standard deviations(RSDs)of 2.9%~8.1%.The method was easy,fast,highly sensitive and fine reproducibility,and was suitable for the determination of tulathromycin and its metabolite in pig tissues.