CAJ | 학술논문

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,1.7μm )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1～100μg/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0.1~0.2μg/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。
목적：건립동시측정유제품중β-내선알항생소(두포고동、두포새우)급기억제제(서파탄、타서파탄)적초고압액상색보-천련질보분석방법。방법양품경을정침정단백,정기완거제지방후,채용Oasis HLB고상췌취주진일보정화,득도양품용액。이Waters UPLC BEH C18주(50 mm×2.1 mm,1.7μm )분리,채용전분무부리자모식전리(ESI-),다반응감측(MRM)모식검측,이보류시간화량대MRM리자대적비정성,기질필배곡선정량。결과4충분석물재1～100μg/L범위내성선성,상관계수r>0.997,공백양품중4충분석물적첨가회수솔위85.5%~95.5%,검출한위0.1~0.2μg/L。결론본방법쾌속、령민,중현성호,가용우유제품중β-내선알류항생소급기매억제제적쾌속준학검측。
Objective An ultra pressure liquid chromatography (UPLC) tandem mass spectrometric (MS/MS) me-thod 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 ex-tracted 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, 1.7μm), 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 re-peatable, and it could be performed for the determination ofβ-lactam antibiotics andβ-lactamase inhibitors in milk-marix.