CN105116076A - Method for detecting cefodizime sodium related substances - Google Patents

Abstract

The invention relates to a method for detecting cefodizime sodium related substances. Ammonium dibasic phosphate and acetonitrile are served as mobile phases to perform gradient elution; and cefodizime can be effectively separated from the related substances.

Description

A kind of detection method of Cefodizime Sodium related substance

Technical field

The present invention relates to a kind of detection method of Cefodizime Sodium related substance.

Background technology

Cefodizime Sodium (cefodizime) is as third-generation cephalosporin, in the world first by German HoechstRoussel Developed, go through in Japan's listing (trade name: Neucef) in nineteen ninety, within 1994, go through in importer, domestic and international clinical practice has the history of nearly 20 years.

The known at present impurity of this product is: 2-sulfydryl-4-methyl-5-thiazole acetic acid (related substance I) and Δ-2 Cefodizime (related substance II).

The existing liquid phase testing conditions of Cefodizime Sodium is mixed into mobile phase with 920:80, isocratic elution with phosphate buffer (get potassium dihydrogen phosphate 0.87g and ADSP 0.22g, be dissolved in water and be diluted to 1000ml, shaking up) and acetonitrile.Though the method can realize effectively being separated of Cefodizime and related substance, be difficult to tackle the separation of complicated ingredient under the accelerated test conditions such as acid, alkali, high temperature.

Summary of the invention

The present invention relates to a kind of new method that Cefodizime Sodium related substance is detected:

Need testing solution: get cefodizime sodium for injection appropriate, dissolves with water for injection and is quantitatively diluted to the solution of 0.5mg/ml;

Mobile phase A: 5mmol/L ammonium dibasic phosphate solution;

Mobile phase B: acetonitrile;

Chromatographic column: 200mm × 4.6mm, 5 μm;

Filler: C18 alkyl silane bonded silica gel;

Column temperature: 25 DEG C;

Determined wavelength: 262nm;

Flow velocity: 1.0mL/min;

Condition of gradient elution:

Time/min	Mobile phase A (%)	Mobile phase B (%)
			0	95	5
15	80	20
			20	80	20
25	95	5
			30	95	5

Get above-mentioned need testing solution 20 μ l, inject high performance liquid chromatograph, record chromatogram.

Adopt detection method of the present invention can realize effectively being separated of Cefodizime Sodium and related substance I, related substance II and trans Cefodizime, degree of separation is good, and has good reappearance.

Accompanying drawing explanation

Fig. 1 adopts detection method of the present invention Cefodizime Sodium to be detected to the liquid chromatogram obtained.

Embodiment

Need testing solution: get cefodizime sodium for injection appropriate, dissolves with water for injection and is quantitatively diluted to the solution of 0.5mg/ml;

Mobile phase A: 5mmol/L ammonium dibasic phosphate solution;

Mobile phase B: acetonitrile;

Chromatographic column: 200mm × 4.6mm, 5 μm;

Filler: C18 alkyl silane bonded silica gel;

Column temperature: 25 DEG C;

Determined wavelength: 262nm;

Flow velocity: 1.0mL/min;

Condition of gradient elution:

Time/min	Mobile phase A (%)	Mobile phase B (%)
			0	95	5
15	80	20
			20	80	20
25	95	5
			30	95	5

Get above-mentioned need testing solution 20 μ l, inject high performance liquid chromatograph, record chromatogram.

Differentiated by the ownership of internal standard method to impurity peaks, result is as follows:

Synergy	RT	Content (%)
			2-sulfydryl-4-methyl-5-thiazole acetic acid	3.280	0.11
Δ-2 Cefodizime	6.477	0.03
			Cefodizime	7.267	99.6
Trans Cefodizime	10.460	0.06

Claims (2)

1. a detection method for Cefodizime Sodium related substance, is characterized in that:

Need testing solution: get cefodizime sodium for injection powder appropriate, dissolves with water for injection and is quantitatively diluted to the solution of 0.5mg/ml;

Mobile phase A: 5mmol/L ammonium dibasic phosphate solution;

Mobile phase B: acetonitrile;

Chromatographic column: 200mm × 4.6mm, 5 μm;

Filler: C18 alkyl silane bonded silica gel;

Column temperature: 25 DEG C;

Determined wavelength: 262nm;

Flow velocity: 1.0mL/min;

Condition of gradient elution:

Get above-mentioned need testing solution 20 μ l, inject high performance liquid chromatograph, record chromatogram.

2. the detection method of Cefodizime Sodium according to claim 1, is characterized in that: differentiated by the ownership of internal standard method to impurity peaks, result is as follows:

。