SPE-UPLC-MS/MS法测定牛奶中β-内酰胺类药物残留

摘要

本试验应用固相萃取技术(SPE),结合超高效液相色谱-串联质谱联用仪(UPLC-MS/MS),建立了快速测定生鲜乳中β-内酰胺类药物残留的方法.样品经乙腈提取,Oaiss PRiME HLB固相萃取小柱净化后,以0.1％甲酸乙腈溶液和0.1％水溶液为流动相,Waters C18色谱柱进行分离;多反应监测(MRM)模式,外标法进行定量.方法回收率在70.1％～95.5％之间;相对标准偏差(n=3)范围为1.0％～9.1％;线性范围为0.002～0.100mg/L;检出限为0.1～～0.6μg/kg;定量限为0.3～1.8μg/kg.表明该方法专属性强、灵敏度高,适用于生鲜乳中β-内酰胺类药物残留的测定.%The samples were extracted by acetonitrile and purified with Oaiss an PRiME HLB cartridge.The UPLC analyses were performed on an Acquity UPLC C18 column with gradient elution using acetonitrile(containing 0.1％ formic)and water(containing 0.1％ formic) as mobile phase.The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring(MRM) in electrospray positive ionization mode.The average recoveries of β-lactams antibiotics ranged from 70.1％ to 95.5 ％,with the relative standard deviation from 1.0％ to 9.1％,the calibration curve was liner from 0.002 to 0.100mg/L,the detection limits of β-1actams antibiotics were 0.1-0.6μg/kg and the limit of quantitation were 0.3-1.8μg/kg.This method is specific,sensitive and suitable for determination of β-lactams antibiotics in the milk.