超高压液相色谱-串联质谱法测定牛奶中的β-内酰胺类抗生素及其酶抑制剂
目的 建立同时测定乳制品中β-内酰胺抗生素(头孢哌酮、头孢噻肟)及其抑制剂(舒巴坦、他唑巴坦)的超高压液相色谱-串联质谱分析方法。方法 样品经乙腈沉淀蛋白, 正己烷去除脂肪后, 采用Oasis HLB固相萃取柱进一步净化, 得到样品溶液。以Waters UPLC BEH C18柱( 50 mm×2.1 mm, 1.7 μm )分离, 采用电喷雾负离子模式电离(ESI-), 多反应监测(MRM)模式检测, 以保留时间和两对MRM离子对的比定性, 基质匹配曲线定量。结果 4种分析物在1?100 μg/L范围内成线性, 相关系数r>0. 997, 空白样品中4种分析物的添加回收率为85.5%~95.5%, 检出限为 0.1~0.2 μg/L。结论 本方法快速、灵敏, 重现性好, 可用于乳制品中β-内酰胺类抗生素及其酶抑制剂的快速准确检测。
Objective An ultra pressure liquid chromatography (UPLC) tandem mass spectrometric (MS/MS) method has been developed for the simultaneous determination of two β-lactam antibiotics (cefotaxime and cefoperazone) and two β-lactamase inhibitors (tazobactam and sulbactam) in bovine milk and infant formula. Methods The analysts were extracted from milk sample with acetonitrile, defatted with liquid-liquid extraction by hexane, and further purified by Oasis HLB solid phase extraction cartridges. The extracted analysts were separated by UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm), and determined by UPLC-MS/MS under negative ionization mode. Results The method showed a good linearity over the range of 1?100 μg/L, with the linear correlation coefficient r>0.997. The mean recoveries for four analysts in bovine milk ranged from 85.5% to 95.5%. The limit of detection was 0.1?0.2 μg/L. Conclusion This method is rapid, sensitive and repeatable, and it could be performed for the determination of β-lactam antibiotics and β-lactamase inhibitors in milk-marix.
标题：超高压液相色谱-串联质谱法测定牛奶中的β-内酰胺类抗生素及其酶抑制剂
英文标题：Simultaneous determination of β-lactam antibiotics and β-lactamase inhibitors in milk by ultra pressure liquid chromatography tandem mass spectrometry
作者：
张立 中国检验检疫科学研究院
李娜思 华东理工大学
冯峰 中国检验检疫科学研究院
王文枝 中国检验检疫科学研究院
杨丙成 华东理工大学
储晓刚 中国检验检疫科学研究院
中文关键词:超高压液相色谱-串联质谱,抗生素酶抑制剂,β-内酰胺类抗生素,乳制品,
英文关键词:ultra-high pressure liquid chromatography-tandem mass spectrometry,β-lactamase inhibitors,β-lactam antibiotics,milk-matrix,
发表日期：2013-11-13
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