Novel technology method for purifying berberine in wild berberis sibirica

A technology of berberine and a new method, applied in the field of purifying berberine, can solve the problems of low extraction rate and low product purity

Inactive Publication Date: 2013-04-17
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the disadvantages of conventional techniques such as low extraction rate and low product purity, and provide a method for utilizing biological enzymolysis, ultrasonic intensified extraction and performing silica gel column chromatography to purify three needles of berberine, in order to achieve the above object , the technical scheme that the present invention adopts is: a kind of new method that utilizes biological enzymatic hydrolysis coupled ultrasonic wave to strengthen extraction, and then combines column chromatography to purify berberine, and its steps are as follows:

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0020] Implementation Case 1: A new method of utilizing biological enzymatic hydrolysis coupled with ultrasonic enhanced extraction, combined with column chromatography to purify berberine, the steps are as follows:

[0021] (1) Enzymolysis:

[0022] 100g is crushed into three needles of 20 mesh, using compound cellulase, the enzyme dosage is 0.2% of the substrate, the enzymatic hydrolysis temperature is 40°C, and kept for 1h:

[0023] (2) Ultrasonic extraction:

[0024] Add 50% ethanol, the ratio of solid to liquid is 1:8, ultrasonic extraction, ultrasonic frequency 50KHZ, ultrasonic time 50min, thin-layer chromatography detection and analysis, recovery of ethanol, to obtain crude extract;

[0025] (3) get coarse powder:

[0026] Heat and dissolve the obtained primary extract with ethanol, adjust its pH value to 2.0 with acid, let stand, filter, wash with water until neutral, concentrate and dry to obtain crude berberine extract powder;

[0027] (4) Silica gel column chrom...

Embodiment example 2

[0035] Implementation case 2: A new method of using biological enzymatic hydrolysis coupling ultrasonic enhanced extraction, combined with column chromatography to purify berberine, the steps are as follows:

[0036] (1) Enzymolysis:

[0037] 100g is crushed into three needles of 30 mesh, using compound cellulase, the enzyme dosage is 0.4% of the substrate, the enzymatic hydrolysis temperature is 45°C, and kept for 2h:

[0038] (2) Ultrasonic extraction:

[0039] Add 60% ethanol, ultrasonic extraction, ultrasonic frequency 70KHZ, solid-liquid ratio 1:9, ultrasonic time 60min, thin-layer chromatography detection and analysis, recovery of ethanol, to obtain a crude extract;

[0040] (3) get coarse powder:

[0041] Heat and dissolve the obtained primary extract with ethanol, adjust its pH value to 2.5 with hydrochloric acid, let stand, filter, wash with water until neutral, concentrate and dry to obtain crude berberine powder;

[0042] (4) Silica gel column chromatography:

...

Embodiment example 3

[0050] Implementation Case 3: A new method of using biological enzymatic hydrolysis coupling ultrasonic enhanced extraction, combined with column chromatography to purify berberine, the steps are as follows:

[0051] (1) Enzymolysis:

[0052] 100g was crushed into three needles of 40 mesh, using compound cellulase, the enzyme dosage was 0.6% of the substrate, the enzymatic hydrolysis temperature was 50°C, and kept for 3 hours;

[0053] (2) Ultrasonic extraction:

[0054] Add 70% ethanol, ultrasonic extraction, ultrasonic frequency 80KHZ, solid-liquid ratio 1:10, ultrasonic time 80min, thin-layer chromatography detection and analysis, recovery of ethanol, to obtain crude extract;

[0055] (3) get coarse powder:

[0056] Heat and dissolve the obtained primary extract with ethanol, adjust its pH value to 2.0 with hydrochloric acid, let stand, filter, wash with water until neutral, concentrate and dry to obtain crude berberine powder;

[0057] (4) Silica gel column chromatograp...

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 belongs to the field of natural organic chemistry, and relates to a method for extracting and purifying berberine from wild berberis roots in great khingan, in particular to a novel method for purifying berberis by a biological enzymolysis, ultrasonic extraction and column chromatography purification combined technique. The method has the advantages that 1, a biological enzymolysis technique is applied to allow that berberine in cells is dissolved out fully; 2, an ultrasonic extraction technique is adopted; the heating time for an effective component is shortened; the activity loss is less; the bioactivity of a product is high; and 3, a silica gel column chromatography and recrystallization purification technique is adopted, so that the purity of the effective component, namely berberine is further increased; the operation is simple and easy; the production cost is lowered greatly; and the method can be applicable to industrial use. According to the method, the biological enzymolysis technique is adopted, the effective component is dissolved out as much as possible, then ultrasonic extraction is conducted, alcohol serves as a solvent, then column chromatography purification is conducted, and finally recrystallization is conducted for secondary purification, so that the purity of berberine is increased to 98.4%.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for extracting and purifying berberine from three wild needles in Daxing'an Mountains, in particular to a method for purifying berberine by using biological enzymolysis, ultrasonic extraction combined with column chromatography purification technology new method. Background technique: [0002] Berberis spinosa, also known as the Northeast Three Needles, is a small deciduous shrub that grows on gravel hillsides at high altitudes. It is produced in Dabald Mountain and Tahe Forestry Bureau of Daxinganling Debuer Forestry Bureau. up to 100 cm. The bark is dark gray-black, with thin longitudinal grooves on the branches; the branches are dark gray-brown, with 5-8 forked thorns at the base of the short branches; the thorns at the lower part of the branches are more forked, thin and sharp, dark gray. Leaves clustered on short branches, obovate, oblanceolate or obovate-...

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): C07D455/03
Inventor 张亚红姚德坤姚德利万莉
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap