亲水作用色谱-串联四极杆质谱测定液态奶中舒巴坦

建立了亲水作用色谱-串联四极杆质谱测定液态奶中微量舒巴坦的分析方法。样品经0.2%乙酸水溶液提取,HLB固相萃取柱净化、富集,以甲酸铵-乙腈为流动相,经Acquity UPLC BEH HILIC色谱柱分离后采用电喷雾质谱多反应监测方式(MRM)扫描,外标法定量。结果表明,舒巴坦的质量浓度在1～100μg/L范围内线性关系良好,r2大于0.99,定量下限为1.0μg/kg。加标水平在1.0～50.0μg/kg范围时,回收率为82%～102%,相对标准偏差(RSD)为1.6%～4.7%。该方法前处理简便快捷、灵敏度高、回收率和重现性良好,适用于液态奶中舒巴坦的测定。

Determination of Sulbactam in Milk by Hydrophilic Interaction Chromatography Tandem Mass Spectrometry(HILIC-MS/MS)

An analytical method was developed for the determination of sulbactam in milk using hydrophilic interaction chromatography tandem mass spectrometry(HILIC-MS/MS).The samples were extracted with 0.2% acetic acid solution,then purified and enriched with an HLB solid-phase extraction(SPE)cartridge.The separation of sulbactam was carried out on an Acquity UPLC BEH HILIC column using ammonium formate-acetonitrile as mobile phase.The quantitation analysis of target compound was performed under the multiple reaction monitoring(MRM) mode by the external standard method.A good linear relationship was obtained between peak area and concentrations of sulbactam in the range of 1-100 μg/L,with correlation coefficients more than 0.99 and limit of quantitation(LOQ) of 1.0 μg/kg.The recoveries at spiked levels of 1.0-50.0 μg/kg ranged from 82% to 102% with relative standard deviations of 1.6%-4.7%.With the advantages of convenience,sensitivity,good recovery and repeatability,the method was suitable for the detection of sulbactam in milk.