论文部分内容阅读
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Themo Hypersil Gold aQ(100 mm ×2.1 mm,1.9 μm)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 ~ 10 μg/L范围内,线性关系良好,方法的定量限为0.5 μg/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 aQ 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.