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李曼琳1,袁耀佐2,姚海燕3,宋〓敏1,杭太俊1
李曼琳1,袁耀佐2,姚海燕3,宋〓敏1,杭太俊1
李曼琳1,袁耀佐2,姚海燕3,宋〓敏1,杭太俊1

1 中国药科大学药物分析教研室,南京 210009;2 江苏省食品药品监督检验研究院,南京 210008; 3 江苏省信诺医药对外贸易有限公司,南京 210019
Identification of the related substances of cefditoren  pivoxil by LC-MS techniques
(1 Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China; 2 Jiangsu Institute for Food and Drug Control,Nanjing 210008,China;3 Jiangsu Xinnuo  Pharmaceutical Foreign Trade Co.,Ltd.,Nanjing 210019,China)

摘要参考文献相关文章

起始页:1770

摘要:目的:采用色谱-质谱联用技术鉴定头孢妥仑匹酯的有关物质,为其工艺优化和质量控制提供参考依据。方法:采用YMC-Pack ODS-AM(150 mm×4.6 mm,5 μm)色谱柱,以甲醇-乙腈-乙酸铵缓冲液为流动相,梯度洗脱,对头孢妥仑匹酯有关物质进行分离;采用电喷雾正离子化-飞行时间质谱法(ESI-TOF/MS)测定各有关物质离子的准确质量和元素组成,三重四极质谱(ESI-MS/MS)测定子离子特征。结果:在所建立的条件下,头孢妥仑匹酯及其有关物质分离良好,检测并鉴定出10个主要有关物质。结论:色谱-质谱联用技术能有效地分离鉴定头孢妥仑匹酯中的有关物质,鉴定结果为其质量控制和工艺优化提供了参考。

关键词:头孢妥仑匹酯;有关物质;降解产物;结构鉴定;色谱-质谱联用

通讯作者:杭太俊,男,教授,博士生导师,主要从事药物分析研究。

基金项目:

作者简介:李曼琳,女,硕士研究生,主要从事药物分析研究。

Abstract:Objective:To identify the related substances of cefditoren pivoxil for its manufacturing process optimization and quality control. Methods:A YMC-Pack ODS-AM(150 mm×4.6 mm,5 μm) column was used for separation of the related substances with a mixture of methanol, acetonitrile, and ammonium acetate buffer as the mobile phase eluted with gradient program. Electrospray positive ionization high resolution TOF/MS was used for the determination of the accurate mass and elemental composition of the parent ions of the related substances,and triple quadrupole tandem mass was employed for the product mass spectra determination. The structures of the related substances were then figured out through elucidation of the fragment ions. Results:Cefditoren pivoxil and the related substances were adequately separated under the established HPLC conditions. Ten major related substances of cefditoren pivoxil were detected and speculated by the hyphenated techniques. Conclusion:The established LC-MS method is effective for separation and identification of the related substances of cefditoren pivoxil and the results of this study are useful for the quality control and process optimization of cefditoren pivoxil.

Key words:cefditoren pivoxil;related substances;degradation products;structure identification;LC-MS

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