目的：建立同时测定乳制品中10种青霉素类抗生素残留的超高效液相色谱-串联质谱分析方法。方法样品经乙腈提取后,乙腈饱和正己烷除去脂肪,经0.22μm 微孔滤膜过滤,用乙腈-水(含0.1%甲酸5 mmol/L乙酸铵)为流动相, C18柱分离,20 min内梯度洗脱分离10种青霉素；电喷雾正离子模式电离(ESI+),多反应监测模式检测(MRM),外标法定量。结果在0.1~20μg/L浓度范围内,10种青霉素类药物在各种乳制品基质中均有良好的线性关系,线性相关系数均＞0.999；液体乳最低检测限为0.2μg/kg~1.0μg/kg,乳粉的最低检测限1.0μg/kg~5.0μg/kg；方法回收率在70.2%~108.2%,相对标准差为＜15%。结论该方法测定乳制品中10种青霉素药物的残留量简便、快速、准确,可以满足对青霉素类抗生素的监测要求。%ABSTRACT:Objective To establish a method for simultaneous determination of 10 residual penicillin in dairy products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with acetonitrile and degreased with saturated acetonitrile n-hexane and filtered through 0.22μm millipore membrane. The filtrate was detected by ultra high performance liquid chromatography-tandem mass spectrometry, identified by electrospray ionization (ESI) in positive mode using multiple reactions monitoring mode, and quantified with external standard method. The sample extract was separated on a C18 column by gradient elution in 20 min with acetronitrile-water (containing 0.1% formic acid and 5 mmol/L ammonium acetate) as mobile phase.Results The calibration curve of the 10 penicillins residues showed a good linearity in the range of 0.1μg/L~20.0μg/L in various dairy products in the matrix with the correlation coefficientr2>0.999. The detection limit of the method was 0.2μg/kg~1.0μg/kg for liquid milk and 1.0μg/kg~5.0μg/kg for milk powder. The recoveries of spiking levels ranged from 70.2% to 108.2%, and the relative standard deviation (RSD) was less than 15%. ConclusionThe method for determination of residues of 10 penicillin antibiotics in dairy products is simple, rapid and accurate, and could satisfy the requirements for monitoring of penicillin residues n requirements for monitoring of penicillin residues
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