UPLC-MS/MS同时测定酱卤制品中15种大环内酯类抗生素

Simultaneous Determination of 15 Macrolide Antibiotics in Sauce Marinated Food Based on UPLC-MS/MS

本研究基于超高效液相色谱-串联质谱建立一种可同时测定15种大环内酯类抗生素的方法。该法能简单、快速的测定酱卤食品中15种大环内酯类抗生素。样品经1%甲酸乙腈超声萃取,采用固相萃取方法净化提取液,采用Agilent ZORBAX SB C 8(2.1 mm×150 mm,3.5μm)作为分离柱,0.1%的甲酸水溶液-甲醇作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式离子化,选择多反应监测(MRM)方式扫描,串联质谱测定,外标法定量。结果显示,各目标物检出限在0.11~0.58μg/kg,相关系数≥0.9994,回收率为82.7%~101.5%,RSD为0.9%~6.2%。本研究前处理操作简单,提取时间较短,回收率稳定,灵敏度高,能够对低浓度的样品进行很好的定性确认,满足对该类药物残留限量的检测要求。

An UPLC-MS/MS method was developed for the simultaneous determination of 15 kind of macrolide antibiotics in leisure food,which could achieve simple and rapid determination of 15 macrolide antibiotics.The sample was extracted by ultrasonic extraction of 1%formic acid acetonitrile,and the extract was purified by solid phase extraction.The separation was performed on Agilent ZORBAX SB C 8(2.1 mm×150 mm,3.5μm)column with a gradient mobile mixture composed of water containing 0.1%fomic acid and methanol,and the electrospray ionization(ESI)source in positive ion mode was used multiple reaction monitoring(MRM),then tandem MS was used for the measurement,and the external standard method was for the quantification.The measurement results suggested that the detection of the developed method was in a range of 0.11~0.58μg/kg,with an above 0.9994 correlation coefficient.The average recovery rates of 15 macrolide antibiotics across three spike level were 82.7%~101.5%,with relative standard deviation(RSD)of 0.9%~6.2%.In this study,the results of simple pretreatment operation,shorter extraction time,stable recovery rate,high sensitivity.and qualitatively confirming the low concentration samples,could meet the detection requirements of the residue limits of this kind of drugs.