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Detection method of azithromycin related substances

A technology of azithromycin and detection method, applied in the field of drug detection, which can solve the problems of inability to separate and measure known impurities and inability to carry out strict quality control

Active Publication Date: 2021-05-18
BEIJING YUEKANGKECHUANG PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the existing azithromycin impurity detection method cannot effectively separate and measure 19 known impurities in azithromycin, and cannot carry out strict quality control

Method used

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  • Detection method of azithromycin related substances
  • Detection method of azithromycin related substances
  • Detection method of azithromycin related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] This embodiment provides a method for the determination of related substances of azithromycin by high performance liquid chromatography, which is determined by the method of chromatographic conditions:

[0068] Chromatographic column: use octadecylsilane bonded silica gel as filler, choose Waters ShieldRP18, 4.6mm×250mm, 3.5μm chromatographic column;

[0069] Mobile phase A: 0.05mol / L dipotassium hydrogen phosphate solution (adjust the pH value to 8.20-8.25 with 20% phosphoric acid solution)-acetonitrile (98:2);

[0070] Mobile phase B: acetonitrile-methanol (90:10);

[0071] Column temperature: 45~48℃;

[0072] Detection wavelength: 210nm; injection volume: 50μL

[0073] Flow rate: 0.8mL / min;

[0074] Solvent: Take 1.73g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000ml, adjust the pH value to 10.0 with ammonia test solution)-methanol-acetonitrile (35:35:30);

[0075] Gradient elution was used.

[0076] The program of gradient elution ...

experiment example 1

[0086] Experimental Example 1 System Suitability Test

[0087] Preparation of each impurity positioning solution: Accurately weigh azithromycin impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity G, impurity H, impurity I, impurity J, impurity K, impurity L, impurity M, Impurity N, Impurity O, Impurity Q 1 , impurity Q 2 19 impurities such as impurity R, impurity S, and the appropriate amount of azithromycin reference substance, add solvent respectively (ammonium dihydrogen phosphate 1.73g, add water to dissolve and dilute to 1000ml, adjust the pH value to 10.0 with ammonia test solution)-methanol-acetonitrile ( 35:35:30)) dissolved and diluted to make G, D, K, Q EP (Q 2 ) four known impurities are all 20μg / mL, other impurities A, F, J, N, O, P, Q (Q 1 ), the concentrations of S, C, E, H, I, L, M, and R are all 50 μg / mL, and the concentration of the azithromycin is 10 mg.

[0088]Preparation of the test solution: Take about 100 mg of azithromy...

experiment example 2

[0110] Experimental example 2 linearity and range test

[0111] Solvent: (1.73g of ammonium dihydrogen phosphate, dissolved in water and diluted to 1000ml, adjusted to pH 10.0 with ammonia test solution)-methanol-acetonitrile (35:15:50)).

[0112] Linear sample solution: Accurately weigh azithromycin impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity G, impurity H, impurity I, impurity J, impurity K, impurity L, impurity M, impurity N, Impurity O, Impurity Q 1 , impurity Q 2 , impurity R, impurity S and azithromycin reference substance in appropriate amounts, respectively add solvent to dissolve to make each stock solution, accurately measure appropriate amount, dilute with solvent to form a series of linear sample solutions, shake well, and obtain.

[0113] Accurately measure 50 μL of each of the above solutions, inject them into a liquid chromatograph, and record the chromatograms. The results are shown in Table 3.

[0114] Table 3 Linearity...

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Abstract

The invention provides a detection method of azithromycin related substances. The detection method comprises the following steps: carrying out detection by adopting a high performance liquid chromatography, taking octadecylsilane chemically bonded silica as a stationary phase, taking a mixed solution of a mobile phase A and a mobile phase B as a mobile phase, and detecting a sample to be detected in a gradient elution manner, wherein the mobile phase A is a mixed solution of a water phase and acetonitrile, and the mobile phase B is a mixed solution of acetonitrile and methanol. According to the method provided by the invention, 19 known impurities in azithromycin can be effectively separated and determined, and strict quality control is carried out.

Description

technical field [0001] The invention relates to the field of drug detection, in particular to a method for detecting related substances of azithromycin. Background technique [0002] Azithromycin is a macrolide drug that was discovered in 1980 and launched in 1981. Azithromycin is a broad-spectrum antibiotic obtained by modifying the structure of erythromycin. Like roxithromycin, it belongs to the second generation of macrolide antibiotics. It is suitable for respiratory tract, skin and soft tissue infections caused by sensitive bacteria, and chlamydia. causing spread of disease. Azithromycin was first developed and synthesized by the Croatian company Priva, and it was first marketed in the former Yugoslavia. The original research and development company transferred the production and market development rights to Pfizer of the United States and Sigma-Tau of Italy for global development. After Pfizer obtained the global development rights, its approved azithromycin trade n...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/06G01N30/86
CPCG01N30/02G01N30/34G01N30/06G01N30/8679Y02A50/30
Inventor 宋更申李中伟高金双
Owner BEIJING YUEKANGKECHUANG PHARM TECH CO LTD
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