The Quality Research Of Cefmenoxime Hydrochloride Drug Substance And Its Sterillizer Powder For Injection And Isepamicin Sulfate And Its Injection

This subject for the national drug quality standardswas issued by the State Pharmacopoeia Committee of China. The objective of this study was to improve the quality standards of cefmenoxime hydrochloride drug substance and its sterillized powder for injection, and isepamicin sulfate and its injection.It provides a scientific basis for increasing and revising the quality control project of Chinese Pharmacopoeia.The first part of the thesis develops a gradient HPLC method for the determination of related substances of cefmenoxime hydrochloride drug substance and its sterillized powder for injection.Chromatographic behavior and spectral characteristics of cefmenoxime and impurities were studied. Meanwhile, the study investigates and selects the optimum conditions of mobile phase, gradient elution program and measurement wavelength, and establishes the methodology validation. The second partdevelopsa HPLC-ESI-MSn method forseparating and identifying the twelve impurities in cefmenoxime hydrochloride. The structures of the twelve impurities were deduced based on the HPLC-MSn databy use of electrospray ion trap mass spectrometry in the multi-stage MS full scan mode, assisted by the UV spectra and stress testing.The third part develops a cluster analysis methodfor rapid and nondestructive determination of cefmenoxime and water content in cefmenoxime hydrochloride for injection.Cefmenoxime hydrochloride for injections were divided into calibration and validation groups. Then, the quantitative models were established using partial least square through selection of different wavelength ranges, preprocessing methods. The method provides a technical support for anti-counterfeiting in site of drug regulatory system.The fourth part develops a gradientHPLC-ESLD method for the determination of isepamicin sulfate and its injection. The optimal chromatography conditions and detector conditions were studied, and the methodology validation was established.The fifth part establishes a capillary gas chromatographicmethod for determination of the residual in isepamicin sulfate. Theoptimum conditions of sampling modes, chromatographic column, column temperature and solvent were selected, andthe methodology validation was established.