Quality control method of cefixime

Abstract

The invention discloses a quality control method of cefixime. Octadecyl silane bonded silica gel is adopted as the chromatographic column of filler, and the detection conditions are as follows: mobilephase: phase A: tetrabutyl ammonium hydroxide aqueous solution (pH 6.5) and acetonitrile in a ratio of 50:50, phase B: tetrabutylammonium hydroxide aqueous solution (pH6.5) and acetonitrile in a ratio of 85:15, column temperature: 0-50DEG C, sample size: 5-25microL, sample introduction concentration: 0.0005-2mg / mL, flow rate: 0.8-1.5ml / min, and detection wavelength: 254nm. The method provided bythe invention can achieve effective separation and quantitative detection of unknown impurities undetectable in the prior art, and the detection efficiency and detection accuracy are both higher thanthose of the prior art. The method has high universality, and can be widely applied to quality detection of cefixime bulk drugs from different sources and corresponding preparations thereof.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a quality control method for a cefixime raw material drug and a preparation. Background technique [0002] Cefixime (Cefixime, CAS: 79350-37-1), a third-generation oral cephalosporin antibiotic, is mainly used clinically to treat pharyngitis, tonsillitis, acute bronchitis, otitis media, urethra caused by sensitive bacteria infection, etc. Cefixime has the characteristics of spectrum, high efficiency and long half-life. Its structural formula is as follows: [0003] [0004] The adverse drug reaction represented by immediate antibiotic allergy is a phenomenon that needs to be strictly controlled and avoided in the clinical use of antibiotics, and the related substances contained in the API are one of the important causes of a series of adverse drug reactions. Therefore, the analysis and research of related substances in APIs and corresponding preparations are very important. [...

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Problems solved by technology

[0006] Specifically, the United States Pharmacopoeia (USP 41), the Chinese Pharmacopoeia (2015 edition), the European Pharmacopoeia (EP 9.0) and the Japanese Pharmacopoeia have all recorded the analytical methods of the raw materials and preparations of cefixime, which all adopt acetonitrile-tetrabutyl hydroxide The ammonium buffer aqueous solution system is used as the mobile phase, and the method of elution with a fixed ratio mobile phase is adopted. The elution time is about 45 minutes (3 times the retention time of cefixime). This method can realize the quantitative detection of conventional related substances, but for special unknown Poor detection of impurities

[0007] "Journal of Pharmaceutical Analysis", Bian Lei et al., 2010, 30 (5), P872 discloses a method for analyzing related substances in cefixime by acetonitrile-assisted electrospray LC-MS / MS method. The method uses 1% formic acid aqueous solution- Acetonitrile (90:10A)-acetonitrile (B) is used as the mobile phase, and the gradient elution method is used to realize the elution and separation of active ingredients and related substances. The elution time is 40 minutes. This method can realize the quantification of 21 common related substances However, for special unknown impurities, due to the short elution time, the resolution and / or peak shape of some impurities is not good, and even some cases cannot be detected, and the comprehensive detection effect is still not good

[0008] "Chromatography", Zhang Xiuyao et al., 2014, 32(7), P693 discloses a method for the determination of β-lactam antibiotics and their metabolite residues in milk by ultra-high performance liquid chromatography. The method uses an aqueous solution-acetonitrile system As the mobile phase, the method of gradient elution is adopted, and the elution time is 10 minutes. However, this method only realizes the separation of the peaks of each antibiotic and its metabolites, and cannot realize the detection of related substances with a small content.

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