Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for measuring related substances of azithromycin capsule by high performance liquid chromatography

A technology of high-performance liquid chromatography and azithromycin gel, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as the inability to realize the determination of azithromycin capsules

Active Publication Date: 2019-06-11
BEIJING YUEKANGKECHUANG PHARM TECH CO LTD
View PDF5 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, azithromycin can be made into various preparation forms, such as capsules, injections, eye drops, etc. The prior art discloses methods for determining the related substances of azithromycin eye drops and injections. The methods disclosed above cannot detect the related substances in azithromycin capsules. Therefore, it is necessary to provide a method for the determination of related substances in azithromycin capsules

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for measuring related substances of azithromycin capsule by high performance liquid chromatography
  • Method for measuring related substances of azithromycin capsule by high performance liquid chromatography
  • Method for measuring related substances of azithromycin capsule by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0041] Experimental Example 1 System suitability test

[0042] Preparation of mixed control solution: take appropriate amount of impurities A, B, C, E, F, G, H, I, J, L, M, N, Q, R, S and azithromycin, add diluent (diluent is the volume ratio) It is a 7:7:6 ammonium dihydrogen phosphate solution (weigh 1.73 g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000 mL, adjust the pH value to 10.0±0.1 with ammonia test solution, a mixture of methanol and acetonitrile,) dissolve and dissolve Dilute to prepare a solution containing 10 mg of azithromycin per 1 mL and 0.05 mg of each impurity as a mixed control solution.

[0043] The preparation of each impurity positioning solution: take the appropriate amount of impurities A, B, C, E, F, G, H, I, J, L, M, N, Q, R, S, respectively add the diluent to dissolve and dilute to make Each 1 mL solution containing 0.05 mg of the above impurities was used as the impurity positioning solution.

[0044] Preparation of the...

experiment example 2

[0054] Experimental example 2 Linearity and range test

[0055] Stock solution of each impurity solution: Precisely weigh 10 mg each of impurities A, B, C, E, F, G, H, I, J, L, M, N, Q, R, and S, and place them in different 5mL volumetric flasks, respectively. Add an appropriate amount of diluent, ultrasonically dissolve it, add diluent to dilute to the mark, shake well, and use as impurities A, B, C, E, F, G, H, I, J, L, M, N, Q, R, S solution stock solution.

[0056] Azithromycin reference substance stock solution: Accurately weigh 10 mg of azithromycin reference substance, put it in a 5mL volumetric flask, add an appropriate amount of diluent, dissolve by ultrasonic, add diluent to dilute to the mark, and shake well.

[0057] Linear solution: Precisely measure 0.5 mL of azithromycin reference stock solution, 0.5 mL of impurity B solution stock solution, 0.1 mL of impurity G solution stock solution, and impurities A, C, E, F, H, I, J, L, M, N 0.25mL of each of the stock so...

experiment example 3

[0077] Experimental example 3 recovery rate test

[0078] Test solution: Accurately weigh an appropriate amount of azithromycin capsule content (equivalent to a prescription ratio of 250 mg of azithromycin), put it in a 25mL volumetric flask, add an appropriate amount of diluent, ultrasonicate for 10 minutes to dissolve azithromycin, let it cool, and add diluent to dilute to the mark , Shake well, filter, take the filtrate, that is. (New system for temporary use)

[0079] Stock solution of each impurity solution: Precisely weigh 10 mg each of impurities A, B, C, E, F, G, H, I, J, L, M, N, Q, R, and S into different 5mL volumetric flasks, respectively. Add an appropriate amount of diluent, ultrasonically dissolve it, add diluent to dilute to the mark, shake well, and use as impurities A, B, C, E, F, G, H, I, J, L, M, N, Q, R, S solution stock solution.

[0080] Recovery rate reference solution stock solution: Precisely measure the above impurity B solution stock solution 0.5...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for measuring the related substances of an azithromycin capsule by high performance liquid chromatography. The method adopts octadecyl silane bonded silica gel as a chromatographic column of filler, and a mobile phase A is characterized in that the ratio of 0.05mol / L of dipotassium phosphate to acetonitrile is 97-99:1-3, wherein the pH value of the 0.05mol / L of dipotassium phosphate is regulated to 8.2 by 20% phosphoric acid solution; and a mobile phase B is acetonitrile, a column temperature is 20-35DEG C, a detection wavelength is 205-215nm, and a flow rate is0.8-1.1mL / min. Since a gradient elution isochromatic spectrum condition is adopted for detection, the method has the advantages of good specificity, high analysis speed and high reproducibility and can be used for accurately and sensitively detecting 15 known impurities and other unknown impurities of the azithromycin capsule, and a related substance chromatography condition is obviously superiorto domestic and oversea pharmacopeia methods.

Description

technical field [0001] The invention belongs to the field of related substance detection, in particular to a method for determining related substances of azithromycin capsules by high performance liquid chromatography. Background technique [0002] Azithromycin (AZM) is a new type of macrolide antibiotic, which is obtained by a series of reactions such as Beckman rearrangement and N-methylation of erythromycin A9-keto oxime. It was developed by Pliva Company in Croatia in 1980 and launched worldwide in 1988. It has been used for more than 30 years. [0003] At present, azithromycin can be made into various preparation forms, such as capsules, injections, eye drops, etc. The prior art discloses methods for measuring the related substances of azithromycin eye drops and injections, and the methods disclosed above cannot realize the determination of related substances in azithromycin capsules. Therefore, it is necessary to provide a method for the determination of related subst...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
Inventor 宋更申安百锋肖佳普张婷婷
Owner BEIJING YUEKANGKECHUANG PHARM TECH CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com