Objective: To establish a method for determination of polymer impurities in cefmenoxime hydrochloride raw materials and preparations. Methods: A high concentration solution was degradated to prepare degradation solution;High performance size exclusion chromatography method（HPSEC,with TSK-gel G2000SWxl column,）and column switching-LC/MSn method were applied to separate and identify the polymer impurities in cefmenoxime hydrochloride degradation solution and evaluate the specificity of HPSEC method;a new RP-HPLC method for polymer analysis was established with an Kromasil 100-5,C18 column,using a mobile phase gradient elution by water-acetonitrile-glacial acetic acid．The specificity of RP-HPLC method was assessed by dimensional chromatography method and column switching-LC/MSn method,and the polymers in samples were analyzed by RP-HPLC method. Results: A series of polymer impurities in cefmenoxime hydrochloride degradation solution were identified including cefmenoxime dimmers and isomers,but no trimers or tetramers were detected． Polymer impurities were liable to co-elute with small molecular impurities by HPSEC method,leading to a poor quantification accuracy and specificity．Cefmenoxime dimer and isomer were detected by RP-HPLC method with a satisfied specificity. Conclusion: HPSEC method is not suitable for the quality control of polymer impurities in cefmenoxime hydrochloride raw materials or productions,while the new established RP-HPLC method is specific, which can effectively control the polymer impurities．Cefmenoxime dimer degradation solution can be used to identify polymer peaks as the system suitability solution.
LI Jin, YAO Shang-chen, YIN Li-hui, XU Ming-zhe, HU Chang-qin
. Analysis of polymer impurities in cefmenoxime hydrochloride raw material and preparations[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(1)
: 169
-179
.
DOI: 10.16155/j.0254-1793.2021.01.21
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