摘要
目的建立LC-MS／MS法测定注射用重组人干扰素ct2b中氨苄西林残留。方法选择阿莫西林为内标，直接沉淀蛋白。采用AgilentEclipse XDB-C18（4．6mm×150mm，5μm）柱，以乙腈-水（甲酸调pH3．1）为流动相进行梯度洗脱。采用电喷雾离子源（ESI），正离子模式，多反应监测（MRM）。氨苄西林、内标监测离子对的m／z分别为350．0／106．1，350．0／192．0和366．0／114．0，366．0／208．0。结果氨苄西林在0．0442-17．6472ng／mL浓度范围内线性关系良好（r=0．9991），最低定量限为0．0442ng／mL，方法回收率在95．26％-102．40％之间，批内、批间RSD分别小于3．71％及6．88％。结论本方法准确可靠，重复性好，灵敏度高，适用于注射用重组人干扰素α2b中氨苄西林残留检测。
Objective To establish an LC-MS/MS method for the determination of ampicillin residue in recombinant human interferon α2b for injection. Methods Using amoxicillin as the internal standard （IS）, the sample was pretreated by simplified protein precipitated. Chromatographic separation was performed on an Agilent Eclipse XDB-C18（4.6mm× 150mm, 5μm） column with the mobile phase of acetonitrile-water （adjust pH to 3.1 with formic acid） by gradient elution. Electrospray ionization （ESI） source was applied and operated in positive mode, ampicillin and amoxicillin （IS） were detected on multiple reaction monitoring （MRM） mode by the transitions from the precursor to the production （m/z350.0/106.1, 350.0/192.0 and 366.0/114.0, 366.0/208.0）. Results For ampicillin, calibration curve was linear in range from 0.0442 to 17.6472ng/mL（r=0.9991）, the limit of quantitation was 0.0442ng/ mL, the method recovery was between 95.26%-102.40%, the RSD of inter- and intra-day precisions were less than 3.71% and 6.88% respectively. Conclusion This method was found to be accurate, good reproducibility and sensitive for determination of ampicillin residue in recombinant human interferon α2b for injection.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2011年第4期288-291,302,共5页
Chinese Journal of Antibiotics
基金
国家科技支撑计划课题(2008BAI54B07)
