Method for extracting hinokiflavone from Cacumen Biotae

A technology of cypress biflavonoids and cypress leaves, applied in the biological field, can solve the problems of large amount of reagents, complicated purification process, and difficulty in industrial production

Inactive Publication Date: 2013-12-18
NANJING BIAOKE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method requires a large amount of reagents, and the purification process is complicated, making it difficult to realize industrial production

Method used

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  • Method for extracting hinokiflavone from Cacumen Biotae

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Experimental program
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Effect test

Embodiment 1

[0018] Take 20kg of Arborvitae leaves and add 10 times the amount of saturated lime water to soak and extract twice. The extract is filtered and ultrafiltered with a hollow cellulose membrane with a molecular weight cut off of 3000. The permeate is then concentrated with a hollow cellulose membrane with a molecular weight cut off of 500. Adjust the pH of the solution to 5 and add it to the D101 macroporous resin column for adsorption. First, take 5 times the column volume of 20% ethanol solution to elute the impurities, and then use 10 times the column volume of 50% ethanol to elute the active ingredients. The eluent is concentrated to adjust the ph3 crystallization. Filter out the crystals and dissolve them with 80% methanol under reflux, concentrate until the alcohol concentration reaches 10%, add to D101 macroporous resin column for adsorption, first take 5 times column volume of 30% ethanol solution to elute impurities, and then wash with 7 times column volume 60% ethanol T...

Embodiment 2

[0020] Take 20kg of Arborvitae leaves and add 5 times the amount of saturated lime water to soak and extract for 3 times. The extract is filtered and ultrafiltered with a hollow cellulose membrane with a molecular weight cut off of 6000. The permeate is then concentrated with a hollow cellulose membrane with a molecular weight cut off of 400. Adjust the pH of the solution to 5 and add it to the AB-8 macroporous resin column for adsorption. First, take 6 times the column volume of 30% ethanol solution to elute the impurities, and then use 7 times the column volume of 60% ethanol to elute the active ingredients. The eluent is concentrated to adjust the pH4 crystallization. Filter out the crystals and dissolve them with 50% methanol under reflux, concentrate until the alcohol concentration reaches 20%, add to the AB-8 macroporous resin column for adsorption, first take 10 times the column volume of 20% ethanol solution to elute impurities, and then use 7 times the column volume of...

Embodiment 3

[0022] Take 20kg of Arborvitae leaves and add 5 times the amount of saturated lime water to soak and extract for 3 times. The extract is filtered and ultrafiltered with a hollow cellulose membrane with a molecular weight cut off of 6000. The permeate is then concentrated with a hollow cellulose membrane with a molecular weight cut off of 400. Adjust the pH of the solution to 5 and add it to the HZ816 macroporous resin column for adsorption. First, take 6 times the column volume of 30% ethanol solution to elute the impurities, and then use 7 times the column volume of 60% ethanol to elute the active ingredients. The eluent is concentrated to adjust the pH4 crystallization. Filter out the crystals and dissolve them with 50% methanol under reflux, concentrate until the alcohol concentration reaches 10%, add to the HZ816 macroporous resin column for adsorption, first take 6 times the column volume of 20% ethanol solution to elute impurities, and then wash with 7 times the column vol...

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Abstract

The invention discloses a method for extracting hinokiflavone from Cacumen Biotae. The method comprises the following steps: 1) pulverizing Cacumen Biotae, adding 5-10 times of saturated lime water for immersion and extraction for 2-3 times, ultrafiltering the extracting solution through an ultrafiltration membrane, and concentrating the filtrate with a nanofiltration membrane to obtain a concentrated solution; 2) regulating the pH value of the concentrated solution to 3-5, adding into a macroporous resin column for adsorption, carrying out gradient elution with an ethanol solution, concentrating the eluate, regulating the pH value to 3-5, and crystallizing; and 3) dissolving the filtered crystal in a 50-80% methanol solution, concentrating until the methanol concentration is 10-30%, adding into a macroporous resin for adsorption, carrying out gradient elution with an ethanol solution, concentrating the eluate for crystallization, recrystallizing the crystal with a 70% ethanol solution, and drying. The method for producing hinokiflavone has the advantages of simple technological operation, low energy consumption and small pollution, and can easily implement industrial production.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a method for extracting cypress biflavone from leaves of oriental cypress. Background technique [0002] Cypress biflavonoids are flavonoids, CAS number 19202-36-9, melting point 353-355°, molecular weight C30H18O10, molecular weight 538.47. Molecular formula: [0003] [0004] Modern studies have found that cypress biflavone has anti-inflammatory, antibacterial and anti-tumor effects. [0005] Through literature search, the preparation method of cypress biflavone mostly adopts chromatography, such as the patent "a preparation method of cypress biflavone", the method disclosed in this patent adopts polyamide chromatographic column separation. This type of method requires a large amount of reagents and a complicated purification process, making it difficult to realize industrial production. Contents of the invention [0006] The technical problem to be solved by th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 张金芳万冬梅
Owner NANJING BIAOKE BIO TECH
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