液质联用法快速分析畜禽肉中多肽类抗生素

A Rapid Analysis of Polypeptide Antibiotics in Livestock and Poultry Meat by Liquid Chromatography Tandem Mass Spectrometry

本文建立了畜禽肉中3种多肽类抗生素药物的简便快捷、可靠灵敏的检测方法。采用EDTA-甲酸铵-甲醇组合沉淀剂和正己烷双相溶剂进行提取净化,下层液体经浓缩和过滤,直接进行分析,无须固相萃取净化。在流动相中添加0.1%的离子对试剂——三氟乙酸,通过反相C18色谱柱保留,获得良好的峰形,UPLC-MS/MS电喷雾正离子模式下分析。优化后的前处理方法能充分去除复杂基质的干扰,特异性好,灵敏度高。定性和定量检测限范围分别为5~10μg/kg和10~25μg/kg之间。基质添加曲线定量的线性良好,相关系数均大于0.9950。在鸡肉中平均添加回收率在86.9%~120.2%。添加回收的重复性和再现性范围分别为1.2%~6.0%和3.3%~5.5%。牛肉中平均添加回收率在89.3%~114.0%。添加回收重复性和再现性范围分别为0.6%~6.0%和1.9%~7.3%。两种基质的RSD均低于10%。

A rapid and simple analytical method was developed to identify 3 polypeptide antibiotics in chicken and beef.The meat was extracted and purified by the EDTA-ammonium formate-methanol precipitator and n-hexane,and the underlying extract was concentrated and filtered before analysis by LC-MS/MS in positive ion mode without purification by SPE.The results showed that the optimized pretreatment method could fully remove the interference of complex matrix with good specificity and sensitivity.The limit of quantitation(LODs)and the limit of quantification(LOQs)varied from 5 to 10μg/kg and 10 to 25μg/kg,respectively.The linearity of matrix-matched addition curves was more than 0.9950.The average recovery of the spiked polypeptides in chicken was in the range from 86.9%to 120.2%with associated RSD values from 1.2%to 6.0%.The inter-day precision was in range of 3.3%to 5.5%,the average recovery of the spiked polypeptides in beef was in the range from 89.3%to 114.0%with associated RSD values from 0.6%to 6.0%,and the inter-day precision was in range of 1.9%to 7.3%.