盐酸头孢他美酯中有关物质的结构鉴定

目的：采用核磁共振法鉴定盐酸头孢他美酯原料药中3个有关物质的结构。方法：首先采用制备色谱分离出盐酸头孢他美酯原料药中的3个杂质，然后采用LC-Q-TOF-MS、LC-Q-TRAP-MS/MS/MS、¹H-NMR、¹³C-NMR、DEPT、¹H-¹H COSY、HSQC、HMBC、IR和UV数据对杂质进行结构鉴定。结果：通过光谱数据分析，鉴定出盐酸头孢他美酯原料药中3个杂质的结构，并进行归属。3个杂质分别为新戊酰头孢他美酯（杂质Ⅰ）、头孢他美酯二聚物（杂质Ⅱ）、8-（1-硫-2-羰基-3-甲氧基-1-异丁烷）-苯并噻唑（杂质Ⅲ），杂质类型主要为聚合以及头孢他美酯合成副产物。结论：该研究鉴定了头孢他美酯原料药中的3个杂质，对头孢他美酯的质量控制具有指导意义。

Objective: To identify and characterize the structures of three impurities in cefetamet pivoxil hydrochloride drug substances by NMR. Methods: Three impurities in cefetamet pivoxil hydrochloride drug substances were obtained by preparative HPLC,and the structures were elucidated and confirmed by spectral data (LC-Q-TOF-MS,LC-Q-TRAPMS/MS/MS, ¹H-NMR, ¹³C-NMR, DEPT, ¹H-¹H COSY, HSQC, HMBC, IR and UV) comprehensively. Results: Based on the spectral data,the structures of three impurities were characterized as pivalyl cefetamet pivoxil (impurity Ⅰ),dimer of cefetamet pivoxil (impurity Ⅱ) and 8-(1-sulfur-2-carbonyl-3-methoxyl-1-isobutane)-benzothiazole (impurity Ⅲ). The impurities include polymerization and synthesis by-product of cefetamet pivoxil. Conclusion: This established method is suitable for the identification of related substances and provides a tool for the quality control of cefetamet pivoxil hydrochloride.

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