Supercharge Your Innovation With Domain-Expert AI Agents!

Method for analyzing impurities in mecobalamine sample

An analysis method, the technology of methylcobalamin, applied in the field of drug analysis, can solve the problems of inaccurate determination of the content of cyanocobalamin and hydroxocobalamin, unstable chemical properties, etc., and achieve the advantages of simple operation, good accuracy and high sensitivity Effect

Pending Publication Date: 2021-06-22
北京斯利安药业有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The methylcobalamin raw material is the effective ingredient of the methylcobalamin sheet, and the methylcobalamin raw material is mainly obtained from the methylation reaction of cyanocobalamin (structural formula 1), therefore, the methylcobalamin raw material contains residual cyanocobalamin, and Due to the unstable chemical properties of methylcobalamin, it will degrade under strong light to generate hydroxocobalamin (structural formula 2). Therefore, hydroxocobalamin and cyanocobalamin are the main impurities of methylcobalamin raw materials, and their content directly affects methylcobalamin. The quality of amine raw materials and methylcobalamin preparations, and the accurate determination of the content of cyanocobalamin and hydroxocobalamin in methylcobalamin raw materials and methylcobalamin preparations are important indicators for correctly evaluating the quality of methylcobalamin raw materials and methylcobalamin preparations. The detection methods of methylcobalamin raw materials and methylcobalamin preparations in some Chinese Pharmacopoeia, United States Pharmacopoeia and Japanese Pharmacopoeia all use the solution containing acetonitrile as the dissolving solvent of the sample and the mobile phase of HPLC separation, methylcobalamin raw material and methylcobalamin preparation Hydroxocobalamin, an impurity, gradually reacts with acetonitrile in a solution containing acetonitrile to generate another impurity, cyanocobalamin, which cannot accurately determine the content of cyanocobalamin and hydroxocobalamin in methylcobalamin raw materials and methylcobalamin preparations

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 analyzing impurities in mecobalamine sample
  • Method for analyzing impurities in mecobalamine sample
  • Method for analyzing impurities in mecobalamine sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Example 1 The recovery verification of the detection method provided by the application

[0090] Sample to be tested: Methylcobalamin raw material.

[0091] Chromatographic conditions: Octadecyl bonded silica gel is used as a filler, and the mobile phase is a mixed solution of 0.03mol / L potassium dihydrogen phosphate and methanol (that is, 0.03mol / L potassium dihydrogen phosphate is mobile phase A, methanol is mobile phase B), the column temperature is 40° C., the detection wavelength is 342 nm, and the solvent is 0.03 mol / L potassium dihydrogen phosphate solution. Gradient elution was carried out under the conditions shown in Table 1 below.

[0092] Table 1 Gradient elution program

[0093]

[0094]

[0095] Solution preparation:

[0096] Impurity stock solution: take hydroxocobalamin acetate and cyanocobalamin, accurately weigh, add solvent (0.03mol / L potassium dihydrogen phosphate solution) to dissolve and quantitatively dilute to make hydroxocobalamin, cyan...

Embodiment 3

[0108] Cyanocobalamin, hydroxocobalamin impurity detection result in the methylcobalamin raw material of embodiment 3

[0109] Chromatographic conditions: Octadecyl bonded silica gel is used as a filler, and the mobile phase is a mixed solution of 0.03mol / L potassium dihydrogen phosphate and methanol (that is, 0.03mol / L potassium dihydrogen phosphate is mobile phase A, methanol is mobile phase B), the column temperature is 40° C., the detection wavelength is 342 nm, and gradient elution is performed under the conditions shown in Table 4 below.

[0110] Table 4 Gradient elution program

[0111]

[0112]

[0113] Preparation of solution: take the methylcobalamin raw material and prepare a test sample with a concentration of 0.5 mg / ml with 0.03 mol / L potassium dihydrogen phosphate solution. Take 20ul and inject into the liquid chromatograph, record the chromatogram as figure 1 Shown, retention time 4.783min is hydroxocobalamin absorption peak, retention time 10.381min is ...

Embodiment 4

[0114] Cyanocobalamin, hydroxocobalamin impurity detection result in embodiment 4 methylcobalamin tablets

[0115] Chromatographic conditions: Octadecyl bonded silica gel is used as a filler, and the mobile phase is a mixed solution of 0.03mol / L potassium dihydrogen phosphate and methanol (that is, 0.03mol / L potassium dihydrogen phosphate is mobile phase A, methanol is mobile phase B), the column temperature is 40° C., the detection wavelength is 342 nm, and gradient elution is performed under the conditions shown in Table 5 below.

[0116] Table 5 Gradient elution program

[0117] time (minutes) Mobile phase A(%) Mobile phase B(%) 0 90 10 10 86 14 35 85 15 45 75 25 55 75 25 55.01 90 10 65 90 10

[0118] Solution preparation: Take methylcobalamin tablets, grind into fine powder, and prepare a sample with a concentration of 0.5 mg / ml (calculated as methylcobalamin) with 0.03mol / L potassium dihydrogen phosphate solutio...

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 discloses a method for analyzing impurities in a mecobalamine sample. The analysis method comprises the following steps: carrying out HPLC separation and detection on a solution I containing a mecobalamin sample to obtain a chromatogram, and obtaining the content of impurities according to the chromatogram, wherein solvent of the solution I is a phosphate solution I; the mobile phase for HPLC separation comprises a mobile phase A and a mobile phase B; the mobile phase A comprises a phosphate solution II; the mobile phase B comprises alcohols; the impurities comprise cyanocobalamin and / or hydroxycobalamin. The analysis system of the analysis method does not contain acetonitrile, the impurity hydroxycobalamin is prevented from reacting in the detection process, the content of hydroxycobalamin and / or cyanocobalamin can be accurately obtained, and the method is high in sensitivity and good in accuracy.

Description

technical field [0001] The application relates to a method for analyzing impurities in methylcobalamin samples, which belongs to the technical field of pharmaceutical analysis. Background technique [0002] The main function of methylcobalamin preparations is to repair damaged nerves, relieve numbness, pain and paresthesia, have a good therapeutic effect on peripheral neuropathy, and have been widely used clinically. The methylcobalamin raw material is the effective ingredient of the methylcobalamin sheet, and the methylcobalamin raw material is mainly obtained from the methylation reaction of cyanocobalamin (structural formula 1), therefore, the methylcobalamin raw material contains residual cyanocobalamin, and Due to the unstable chemical properties of methylcobalamin, it will degrade under strong light to generate hydroxocobalamin (structural formula 2). Therefore, hydroxocobalamin and cyanocobalamin are the main impurities of methylcobalamin raw materials, and their cont...

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
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/74G01N30/8634G01N2030/047
Inventor 肖学菊苏小楠张李丹岳玉荣
Owner 北京斯利安药业有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com