摘要
目的旨在建立头孢克肟制剂中有关物质结构鉴定与定量分析方法。方法采用HPLC-Q-TOF-MS/MS法对主要杂质结构进行分析。建立HPLC法,采用C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-四丁基氢氧化铵溶液为流动相进行梯度洗脱,检测波长为254 nm,柱温为40℃,对头孢克肟制剂进行有关物质检测。结果初步鉴定了头孢克肟制剂中9个杂质,分别为杂质A、B、D、E、F、G、H、头孢克肟亚砜和头孢克肟叔丁酯。在建立的HPLC色谱条件下,头孢克肟及各杂质均能达到基线分离,各有关物质的质量浓度在0.1934~20.03μg·mL^(-1)内线性关系良好,r>0.9990;回收率为98.4%~101.8%(RSD<2.0%)。结论HPLC-Q-TOF-MS/MS技术能初步鉴定头孢克肟制剂的杂质结构,该方法能检测不同厂家头孢克肟片剂、颗粒剂、胶囊剂及干混悬剂中的有关物质。
Objective To establish a method for structural identification and quantitative analysis of related substances in cefixime preparations.Methods The main impurities were identified by HPLC-Q-TOF-MS/MS.Related substances in cefixime were separated on an C_(18)column(250 mm×4.6 mm,5μm)with the mobile phase of acetonitrile-tetrabuthylammonium hydroxide solution and detected at 254 nm.Column temperature was set at 40℃.Results Nine impurities in the preparations of cefixime were identified as impurity A,B,D,E,F,G,H,cefixime sulfoxide and cefixime tert-butyl ester.The method could achieve baseline separation.Impurities E,G and H were linear within the range of 0.1934-20.03μg·mL~(-1),r>0.9990,and the recoveries were 98.4%-101.8%(RSD<2.0%).Conclusion HPLC-Q-TOF-MS/MS technology can preliminarily identify the impurity structure of cefixime preparations.The method can accurately detect the related substances in 26 cefixime preparations with a good specificity and high sensitivity.
作者
闫晓娟
于可欣
栗智
管一娜
李清
YAN Xiaojuan;YU Kexin;LI Zhi;GUAN Yina;LI Qing(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China)
出处
《沈阳药科大学学报》
CAS
CSCD
2024年第2期206-216,226,共12页
Journal of Shenyang Pharmaceutical University
基金
沈阳市中青年科技创新人才支持计划项目(RC190505)。
关键词
高效液相色谱法
头孢克肟制剂
有关物质
飞行时间质谱
high performance liquid chromatography
cefixime preparation
related substance
time of flight mass spectrometry
