Quality control method of cefixime

A quality control method and technology of cefixime, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of poor separation degree and/or peak shape of impurities, poor comprehensive detection effect, and poor detection effect of special unknown impurities And other issues

Active Publication Date: 2018-12-07
GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 gra

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Embodiment 1

[0049] Chromatographic column: Agilent ZORBAX SB-C18, 250×4.6mm, 5μm

[0050] Mobile phase:

[0051] Phase A: Tetrabutylammonium hydroxide aqueous solution: Acetonitrile = 50:50

[0052] Phase B: Tetrabutylammonium hydroxide aqueous solution: Acetonitrile = 85:15

[0053] Column temperature: 40℃

[0054] Injection volume: 20μL

[0055] Injection concentration 1mg / mL

[0056] Flow rate: 1.2mL / min

[0057] Detection wavelength: 254nm

[0058] The quality control method of described cefixime comprises the following steps:

[0059] 1. Prepare the solution;

[0060] Take 25mL of 10% tetrabutylammonium hydroxide solution, add purified water to dilute to 1000mL, shake well, adjust pH to 6.5 with 1.5mol / L phosphoric acid solution to obtain tetrabutylammonium hydroxide aqueous solution; mix the corresponding amount of tetrabutylammonium hydroxide aqueous solution with acetonitrile , to obtain A phase and B phase, respectively;

[0061] Take 5 cefixime dispersible tablets (50mg s...

Embodiment 2

[0068] Chromatographic column: Agilent ZORBAX SB-C18, 250×4.6mm, 5μm

[0069] Mobile phase:

[0070] Phase A: Tetrabutylammonium hydroxide aqueous solution: Acetonitrile = 50:50

[0071] Phase B: Tetrabutylammonium hydroxide aqueous solution: Acetonitrile = 85:15

[0072] Column temperature: 40℃

[0073] Injection volume: 20μL

[0074] Injection concentration 1mg / mL

[0075] Flow rate: 1.2mL / min

[0076] Detection wavelength: 254nm

[0077] The quality control method of described cefixime comprises the following steps:

[0078] 1. Prepare the solution;

[0079] Take 25mL of 10% tetrabutylammonium hydroxide solution, add purified water to dilute to 1000mL, shake well, adjust pH to 6.5 with 1.5mol / L phosphoric acid solution to obtain tetrabutylammonium hydroxide aqueous solution; mix the corresponding amount of tetrabutylammonium hydroxide aqueous solution with acetonitrile , to obtain A phase and B phase, respectively;

[0080] Take 5 cefixime dispersible tablets (50mg...

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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. [...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 程志伟赵用强
Owner GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD
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