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

Method and apparatus for simultaneously manufacturing ultra pure betulin and highly pure betulinic acid from birch bark

An ultra-high-purity, betulinic acid technology, applied in chemical instruments and methods, separation methods, pharmaceutical formulations, etc., can solve the problems of non-disclosure, high production costs, and high solvent consumption, so as to save solvent usage and improve productivity Effect

Inactive Publication Date: 2012-11-07
骨碌碌有限公司
View PDF10 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These include the use of pure polar solvents and reflux extraction methods to obtain crude extracts (crude extract), the use of non-polar solvents hexane and polar solvent ethyl acetate to remove non-polar substances, usually filled with silica gel Open column isolation (isolate) of betulin with a purity of 95% or less, but there is no disclosure of a technology capable of continuously producing products with a purity of 99%
[0006] In addition, in the existing crystallization technology, after dissolving the crude extract in a single polar solvent (such as alcohol such as isopropanol) at a temperature near the boiling point, the solubility difference caused by lowering the temperature is used to obtain the Crystal betulin purity is 90%, lower
In addition, the recrystallization method using a single solvent has a disadvantage of high solvent consumption and low crystallization efficiency compared to the case of using a mixed solvent, resulting in high production costs.
[0007] In addition, in the prior art described above, a polar and nonpolar mixed solvent is used to remove nonpolar components, thereby using a large amount of solvent, or a single open column (single open column) filled with a polar stationary phase is used, so the At the technical stage of discontinuous production of betulin with a purity of 95%

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 and apparatus for simultaneously manufacturing ultra pure betulin and highly pure betulinic acid from birch bark
  • Method and apparatus for simultaneously manufacturing ultra pure betulin and highly pure betulinic acid from birch bark
  • Method and apparatus for simultaneously manufacturing ultra pure betulin and highly pure betulinic acid from birch bark

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] HPLC analysis of betulin and betulinic acid (calibration curve)

[0090] Utilizing the technology of the present invention, the concentrations of the crude extract, primary crystals, ultra-high purity betulin and high-purity betulinic acid are utilized figure 2 with image 3 The calibration curve (calibration curve) of betulin and betulinic acid was used for quantitative analysis. Betulin (Sigma: B8795, not less than 98%) and betulinic acid (Sigma: 855057, not less than 90%) were used as standard samples. Dissolve 100 mg of betulin as a standard sample in 20 mL of HPLC grade ethanol at room temperature to prepare a mother solution with a concentration of 5.0 g / L, and dilute the mother solution to obtain a concentration of 4.0 g / L and 3.0 g / L , 2.0 g / L samples were analyzed by HPLC. Dissolve 10 mg of betulinic acid as a standard sample in 20 mL of HPLC grade ethanol to prepare a 0.5 g / L mother solution for analysis, and dilute the mother solution to prepare 0.4 g / L, ...

Embodiment 2

[0092] Production of Crude Betulin Alcohol Extract from Betula Pulpwood Using Ethyl Acetate

[0093] The inner bark and outer bark of birch birch that grow naturally in North America were dried and pulverized so that the moisture content was 6%, and then 150 g of particles under 8 mm and 1900 mL of ethyl acetate were filled in a reflux extraction tank (the unit of outer bark per kg 12.67L), heated at 62°C for 1 hour and at 77°C for 3 hours under atmospheric pressure to extract betulin and betulinic acid into the organic solvent. The mixture contained in the reflux extraction reactor was subjected to high-temperature filtration (hot filtering) at 70° C. with a 0.5 μm PTFE membrane to prevent the solidification of betulin and simultaneously separate the organic solvent from the wet bark. 80% of the total volume of the filtrate was evaporated and the concentrated solution was left at -2°C for 10 hours to crystallize betulin. Betulin crystals obtained by filtering a mixture of be...

Embodiment 3

[0096] Production of Crude Betulin Alcohol Extract from Betula Paperbark Using Chloroform

[0097]Put 178 g of birch inner and outer bark (particle size below 8 mm, moisture content 5%) that mainly grows naturally in North America into a reflux extraction tank filled with 1900 mL of chloroform (10.67 L of chloroform per kg of outer bark). Heating at 49° C. for 1 hour, followed by heating at 61.2° C. for 2 hours, extracted betulin and betulinic acid into the organic solvent. In order to prevent solidification of crystals, the mixture contained in the extraction reactor was filtered at a temperature near the boiling point of chloroform. The organic solvent + extract was separated from the bark, 80% of the filtrate was evaporated, cooled at room temperature, and then left at -2°C for 10 hours to crystallize betulin and betulinic acid. The solid crystals obtained by filtering the crystals with a 0.5 μm PTFE membrane were dried at 35°C (primary crude extract), and 80% of the total...

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
Densityaaaaaaaaaa
Login to View More

Abstract

The present invention relates to a method and apparatus for simultaneously manufacturing ultra pure betulin and highly pure betulinic acid from birch bark, which employ a technique of: using a polar organic solvent to obtain a crude extract containing a betulin content of 70 to 83% and a betulinic acid content of 4 to 8% from the outer bark and inner bark of birch trees that grow naturally in northern hemisphere regions at a northern latitude of 34 DEG or greater, such as in South Korea, China, North America, and Europe; and using a single or mixed polar solvent to obtain a crystallized highly pure betulin with a purity of 95% or greater, wherein ultra pure betulin with a purity of 99.5% or greater and highly pure betulinic acid with a purity of 95% or greater can be simultaneously produced from the crystallized product.

Description

technical field [0001] The present invention relates to a method and a device for simultaneously producing ultra-high-purity betulin and high-purity betulinic acid from birch bark, and relates to the extraction of high-purity betulin from crude extracts obtained from the outer bark and inner bark of birch using a mixture of polar organic solvents. Alcohol is crystallized and the polar pigment components are separated by using eluent change 4-tower continuous adsorption separation, so that ultra-high-purity betulin and high-purity betulinic acid can be produced continuously from birch bark. Ultra-high-purity betulin and high-purity betulin Method and device for purifying betulinic acid. Background technique [0002] It has been published in many documents that betulin is often used as a raw material for organic synthesis of betulinic acid, betulonic acid, or their derivatives, which are effective as therapeutic agents. material (starting material). [0003] The scientific d...

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): A61K36/185B01D11/00B01D9/00
CPCB01D15/1864A61K2236/39A61K36/185B01D9/00B01D11/00
Inventor 朱国铎朴钟基金台焕李昌根
Owner 骨碌碌有限公司
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