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

Cobamamide crystal form and preparation method and application thereof

A technology of adenosylcobalamin crystal and adenosylcobalamin, which is applied in the field of adenosylcobalamin crystal form and its preparation, can solve the problem that the adenosylcobalamin raw material is not completely dissolved, and achieve the effect of uniform particle size

Active Publication Date: 2017-10-10
ZHENGZHOU UNIV +1
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] (3) When repeating the patented method, it was found that the adenosylcobalamin raw material was not completely dissolved, and the experimental process had almost no effect on reducing impurities
Through the study of recrystallization technology, we have obtained a method to obtain a new crystal form with a higher yield and further reduce the impurity of adenosylcobalamin. At present, there is no report of a similar method

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
  • Cobamamide crystal form and preparation method and application thereof
  • Cobamamide crystal form and preparation method and application thereof
  • Cobamamide crystal form and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0077] Under red light lighting conditions, at room temperature. Add 1 g of commercially available adenosylcobalamin to 7ml of water, stir for 5 minutes until it becomes a paste, keep stirring, add 3.5ml of acetone to the above paste, and within 1 minute, adenosylcobalamin is completely dissolved to obtain a clear solution. Add 35ml of isopropanol to the above solution, while stirring for 5min, the stirring rate is controlled at 400r / min, and the system is cloudy at this time. Then, let stand overnight at room temperature, suction-filter the precipitated crystals, wash the filter cake with isopropanol (3*10ml), and vacuum-dry at 25°C for 7 hours to obtain 0.982g of crystal form C adenosylcobalamin with a yield of 98.2%.

[0078] The X-powder diffraction pattern of obtained C crystal form adenosylcobalamin and Figure 4 Consistent, the TG-DSC spectrum is consistent with Figure 9 unanimous. Content analysis was carried out according to the detection method of Chinese Pharmac...

experiment example 2

[0080] Under red light lighting conditions, at room temperature. Add 10 g of commercially available adenosylcobalamin to 60ml of water, stir for 10 minutes until it becomes a paste, keep stirring, add 24ml of acetone to the above paste, within 3 minutes, adenosylcobalamin is completely dissolved to obtain a clear solution. Add 156ml of isopropanol to the above solution, and stir for 5 minutes at the same time, the stirring rate is controlled at 300r / min, and the system is cloudy at this time. Then, let stand overnight at room temperature, suction-filter the precipitated crystals, wash the filter cake with isopropanol (3*20ml), and vacuum-dry at 25°C for 7 hours to obtain 9.930g of crystal form C adenosylcobalamin with a yield of 99.3%.

[0081] The X-powder diffraction pattern of obtained C crystal form adenosylcobalamin and Figure 4 Consistent, the TG-DSC spectrum is consistent with Figure 9 unanimous. Content analysis was carried out according to the detection method of...

experiment example 3

[0083] Under red light lighting conditions, at room temperature. Add 50 g of commercially available adenosylcobalamin to 250ml of water, stir for 30 minutes until it becomes a paste, keep stirring, add 75ml of acetone to the above paste, within 10 minutes, adenosylcobalamin is completely dissolved to obtain a clear solution. Add 250ml of isopropanol to the above solution, while stirring for 1min, the stirring rate is controlled at 100r / min, at this time the system gradually becomes cloudy. Then, let stand overnight at room temperature, suction-filter the precipitated crystals, wash the filter cake with isopropanol (3*50ml), and vacuum-dry at 25°C for 7 hours to obtain 49.200g of crystal form C adenosylcobalamin with a yield of 98.4%.

[0084] The crystal grain size obtained under this condition can reach 0.2 mm, which can be used for X-single crystal diffraction detection. The single crystal diffraction pattern is shown in image 3 , the X-powder diffraction pattern of the ob...

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

No PUM Login to View More

Abstract

The invention relates to a cobamamide crystal form and a preparation method and application thereof. Cu-Ka target radiation is used, and the powder diffraction of X-ray has the characteristic peak at the diffraction angle 2Theta=5.1+ / -0.1, 6.3+ / -0.1, 7.0+ / -0.1, 7.6+ / -0.1, 8.0+ / -0.1, 8.6+ / -0.1, 9.4+ / -0.1, 13.2+ / -0.1, 13.8+ / -0.1, 15.0+ / -0.1, 17.5+ / -0.1, 19.1+ / -0.1, 21.4+ / -0.1, 23.5+ / -0.1, 25.3+ / -0.1. According to the method, a latent solvent is used for dissolving a cobamamide crude product, and a cobamamide refined product is obtained by using an anti-solvent recrystal method. The impurities are remarkably reduced in the preparation process, the operation is simple and convenient, the energy consumption is low, the product purity is higher than 99.5%, the total impurity is less than 0.5%, the yield is greater than 98.0%, and the stability of the product to light, heat and high-humidity is remarkably strengthened. The cobamamide crystal form can be used for the industrial production.

Description

technical field [0001] The invention relates to a crystal form of adenosylcobalamin, a preparation method and application thereof, and belongs to the field of crystallization technology. Background technique [0002] Adenosylcobalamin (Cobamamide also known as Adocbl or Coenzyme B 12 , also known as deoxyadenosylcobalamin), is dark red crystal or powder, very hygroscopic, and easily decomposed when exposed to light. Slightly soluble in water, almost insoluble in ethanol, insoluble in acetone or ether. Its chemical name is 5,6-dimethylbenzimidazolyl-5`-deoxyadenosylcobalamin, and its molecular formula is C 72 h 100 CoN 18 o 17 P, the structural formula is shown in Formula 1. [0003] [0004] At present, adenosylcobalamin is used as a biochemical reagent and experimental reagent in the world, but it is only used as a medicine in my country. It has been used for many years. Adenosylcobalamin was mainly used to treat pernicious anemia in the early stage, and it can al...

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): C07H23/00C07H1/06
CPCC07B2200/13C07H1/06C07H23/00
Inventor 李雯刘宏民郭姗姗施秀芳可钰杨晨周照青李鹏坤李宏
Owner ZHENGZHOU UNIV
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