亲水作用色谱-串联四极杆质谱测定液态奶中舒巴坦  

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

作　　者：薛霞[1] 王骏[1] 刘桂亮[1] 宿书芳[1] 张卉[1] 祝建华[1] 

机构地区：[1]山东省产品质量监督检验研究院,国家加工食品质量监督检验中心(山东),山东省材料化学安全检测技术重点实验室

出　　处：《分析测试学报》2012年第6期700-704,共5页Journal of Instrumental Analysis

摘　　要：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。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.

关 键 词：舒巴坦 亲水作用色谱-串联四极杆质谱 液态奶 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]