新型固相萃取-超高效液相色谱-串联四极杆静电场轨道阱高分辨质谱测定液态乳中舒巴坦  

Determination of sulbactam in liquid milk with new type SPE-Ultra liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry

作　　者：付晓燕 张璐 孔祥虹 何强 李莹 朱振宝[1] 邹阳 李建华 施妍婧 

机构地区：[1]陕西科技大学,西安710021 [2]陕西出入境检验检疫局,西安710068

出　　处：《分析试验室》2018年第3期338-342,共5页Chinese Journal of Analysis Laboratory

基　　金：陕西出入境检验检疫局项目(陕K-201606);国家质检总局项目(2016IK213);陕西省科技资源开放共享平台(2017KTPT-06);陕西省重点研发计划(2017NY-165)资助

摘　　要：建立了新型固相萃取-超高效液相色谱-串联四极杆静电场轨道阱高分辨质谱测定液态乳中舒巴坦的方法。液态乳采用乙腈超声提取后,PRiME HLB固相萃取柱净化。以Thermo Hypersil Gold a Q(100 mm×2.1 mm,1.9μm)色谱柱进行分离,在电喷雾负离子模式下(ESI-),通过优化分辨率,在全扫描模式下提取目标化合物的精确质量数,采用自动触发采集二级质谱图进一步提高定性的准确性。在0.5~10μg/L范围内,线性关系良好,方法的定量限为0.5μg/kg,回收率为82.1%~95.5%,相对标准偏差为3.5%~6.2%。该方法操作简单,测定结果准确,可用于液态乳中舒巴坦残留的测定。A new method to determine sulbactam in liquid milk samples was developed based on new type SPE-ultra liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry after separation with Thermo Hypersil Gold a Q and analysis in negative mode（ESI-）.Samples were extracted by acetonitrile,and then purified by a new type SPE（PRiME HLB）.With the optimized mass resolution,accurate mass measurement of analyte was obtained using full scan mode and twostage threshold-triggered full mass scan mode was utilized to further improve the accuracy of qualitative analysis.The linear range of sulbactam was from 0.5 μg/L to 10 μg/L and the limit of quantification（LOQ） of sulbactam was 0.5 μg/kg.The average spiked recoveries of the method varied from 82.1 % to 95.5 % with relative standard deviations（RSDs） between 3.5 % and 6.2 %.The method is simple and accurate for determination of sulbactam in liquid milk.

关 键 词：PRiME HLB 超高效液相色谱 静电场轨道阱 高分辨质谱 舒巴坦 液态乳 

分 类 号：O657.63[理学—分析化学]