摘要
目的:建立应用高效液相色谱-串联质谱技术快速鉴定头孢地嗪中异构体杂质的方法。方法:以5 mmol.L-1醋酸铵溶液-乙腈为流动相,经C18柱(200 mm×4.6 mm,5μm)分离,通过串联ESI质谱在线检测,获得相关的色谱和质谱信息。结果:在所建立的条件下,头孢地嗪及其异构体杂质获得有效分离,头孢地嗪、反式异构体及Δ3异构体的保留时间分别为11.38,14.26,10.95 min,通过质谱中特征碎片离子的差异可区分反式异构体及Δ3异构体。结论:本法可快速、准确地分离鉴定头孢地嗪中的反式和Δ3异构体杂质,进而可以对药品质量进行质量控制。
Objective:To establish a sensitive and specific LC-MS method for the determination of isomeric impurities in cefodizime.Methods:The HPLC separation experiments were performed on a reversed phase C18 column(200 mm×4.6 mm,5 μm),with 5 mmol·L-1 ammonium acetate-acetonitrile as mobile phase.The analytes were determined by ESI-MS in negative mode.The chromatograms and mass spectra of cefodizime and its isomeric impurities were obtained by LC-MS.Results:The method can be used for the separation and identification of cefodizime and its anti-form,Δ3-cephem form,of which the retention times were 11.38,14.26,10.95 min,respectively.Based on the MS spectra of their molecular ion,the different fragmentation pathways of cefodizime and its isomeric impurities were compared and proposed.Conclusion:The method is rapid,sensitive and specific.It can be used for the identification of the isomeric impurities in cefodizime.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2011年第9期1833-1836,共4页
Chinese Journal of Pharmaceutical Analysis