MEKC和UPLC检测头孢噻吩钠中的3-位置异构体杂质  

Detection of 3-positional isomer impurity in cefalotin sodium by MEKC and UPLC

作　　者：刘浩[1] 秦峰[1] 赵敬丹[1] 丁颖[1] 杨美成[1] 裘亚[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《中国抗生素杂志》2015年第7期516-520,共5页Chinese Journal of Antibiotics

基　　金：重大新药创制专项化学新药质量标准研究与评价技术平台(No.2011ZX09303-001);中国食品药品检定研究院中青年发展研究基金(No.2013WA4)

摘　　要：目的建立并优化检测头孢噻吩钠中3-位置异构体杂质的MEKC法和UPLC法。方法 MEKC法采用非涂层弹性石英毛细管(50μm i.d.,有效柱长为56cm),以含13mmol/L 18-冠-6和0.2mol/L SDS的硼酸盐缓冲液(25mmol/L四硼酸钠溶液,p H9.2)为背景电解质;UPLC法采用苯己基三键键合亚乙基桥杂化颗粒柱(ACQUITY UPLC BEH Phenyl,100mm×2.1mm,1.7μm),以0.05mol/L甲酸铵缓冲液(用甲酸调节p H值至3.0)-乙腈-甲醇(85:9:6)为流动相。结果采用MEKC法,头孢噻吩与其3-位置异构体杂质的分离度可达3.15并基线分离;采用UPLC法二者仅近基线分离且分析时间稍长;MEKC法和UPLC法对同一批供试品的测定结果基本一致。结论采用优化后的MEKC法和UPLC法均可对头孢噻吩钠中的3-位置异构体杂质进行有效的分离和控制。Objective To establish and optimize an MEKC method and an UPLC method for the detection of 3-positional isomer impurity in cafalotin sodium. Methods The MEKC method utilized a bare fused silica capillary （50μm i.d., effective length was 56cm） and a 25mmol/L sodium tetraborate buffer （pH9.2） containing 13mmol/L 18-Crown-6 and 0.2mol/L SDS was used as background electrolyte. The UPLC method utilized a trifunctional phenylhexyl bridged ethylene hybrid column （ACQUITY UPLC BEH Phenyl, 100mm×2.1mm, 1.7μm）, and 0.05mol/L ammonium formate buffer （adjust the pH to 3.0 with formic acid）-acetonitrile-methanol （85：9：6） was used as mobile phase. Results Cefalotin and its 3-positional isomer impurity were baseline separated with the MEKC method. However, they were just nearly baseline separated with the UPLC method, and the analysis time was relatively longer. The results obtained with the MEKC method were consistent with those obtained with the UPLC method for the same batch of sample. Conclusion The optimized MEKC method and UPLC method were both suitable for the separation and control of 3-positional isomer impurity in cefalotin sodium.

关 键 词：MEKC UPLC 头孢噻吩钠 3-位置异构体杂质 

分 类 号：O657.7[理学—分析化学] R978.11[理学—化学]