亲水作用色谱-串联四极杆质谱测定液态奶中舒巴坦

摘要

An analytical method was developed for the determination of sulbactam in milk using hydrophilic interaction chromatography tandem mass spectrometry ( HILJC - 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 (ig/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 conven-ience , sensitivity, good recovery and repeatability, the method was suitable for the detection of sul-bactam in milk.%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1～100 μg/L范围内线性关系良好,r2大于0.99,定量下限为1.0 μg/kg.加标水平在1.0～50.0 μg/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.