2D-LC-IT-TOF/MS联用Cef-SEC法鉴定注射用头孢硫脒中高分子杂质  

Determining the polymers in Cefathiamidine for injection by Cef-SEC two-dimensional UPLC-IT TOF MS method

作　　者：胡卫国 韩彬[1] 胡利敏 高燕霞 王强 张锁庆 HU Weiguo;HAN Bin;HU Limin;GAO Yanxia;WANG Qiang;ZHANG Suoqing(Hebei Institute for Drug Control,Shijiazhuang 050011,China;North China Pharmaceutical Co.,Ltd,Shijiazhuang 050011,China;North China Pharmaceutical Huamin Pharmaceutical Co.,Ltd,China;The School of Chemical Engineering and Thechnology at Tianjing University,Tianjin 300350,China)

机构地区：[1]河北省药品检验研究院,石家庄050011 [2]华北制药股份有限公司,石家庄050011 [3]华北制药河北华民药业有限责任公司,石家庄050011 [4]天津大学化工学院,天津300350

出　　处：《中国药品标准》2020年第5期429-434,共6页Drug Standards of China

摘　　要：目的:建立高效分子排阻色谱法(Cef-SEC)测定头孢硫脒中的聚合物,并用应用在线脱盐-高效液相色谱-离子阱-飞行时间质谱对其聚合物进行结构鉴定。方法:采用WT-Cef-SEC(7.8 mm×30.0 cm,5μm)色谱柱;流动相为5 mmol·L-1磷酸盐缓冲液-乙腈(95∶5);进样量为20μL;检测波长为254 nm;ESI电离源,正离子扫描;主成分自身对照法计算聚合物的含量。结果:在该条件下头孢硫脒峰与聚合物峰分离良好;通过2D-LC-IT-TOF/MS推测出聚合物1为头孢硫脒二聚体,聚合物2为去乙酰头孢硫脒氧化杂质聚合体。结论:本方法适用于注射用头孢硫脒高分子杂质的测定,同时为β-内酰胺类抗生素中聚合物的分离、分析及产品质量提高提供了依据。Objective:To establish a high performance size exclusion chromatography(Cef-SEC)method for determining the polymer in cefathiamidine and its structure identification.Method:The analysis was carried out by using a WT-Cef-SEC chromatography column(7.8 mm×30.0 cm,5μm);The mobile phase was 95 volumes of 5 mmol·L-1 ammonium acetate and 5 volumes of acetonitrile;The detection wavelength was 254 nm;The injection volume was 20μL.The ion source was ESI ionization source,the scan pattern was positive and the content of polymers was determined by main component selfcompare without calibration factor.Results:The polymers were completely separated from cefathiamidine.Polymer 1 was conjectured to be the dimer of cefathiamidine by 2D-LC-IT-TOF/MS.Polymer 2 was conjectured to be the dimer of deacetyl cefathiamidine oxidation.Conclusion:The method has provided basis for the separation and analysis ofβ-lactams polymers,and it can be used to improve the quality of product.

关 键 词：头孢硫脒 高分子杂质 Cef-SEC改良亲水凝胶色谱柱 在线脱盐-高效液相色谱-离子阱-飞行时间质谱 

分 类 号：R921.2[医药卫生—药学]