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Method for extracting genkwanin from Daphne genkwa Sieb.et Zucc.

A technology of genkwain and genkwa, applied in the direction of organic chemistry, can solve the problems of short production cycle, low product purity, and large environmental pollution, and achieve the effects of short production cycle, good adsorption effect, and small environmental pollution

Inactive Publication Date: 2011-09-14
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Raorao et al. used SP850 and SP825 macroporous resins for adsorption treatment and elution with 50% ethanol to investigate the effect of macroporous resin treatment on the HPLC fingerprint of genkwa. In the process, extraction with ethyl acetate, degreasing of petroleum ether, silica gel column chromatography, chloroform-methanol (20:1-1:1) gradient elution, and repeated column chromatography, after multiple Toyopearl HW-40 column chromatography, Gradient elution with water-methanol (1:0-4:6) can finally obtain genkwain. This method has a low extraction rate and uses a large amount of organic solvents. The production cycle is short and it is not suitable for industrial production.
Chu Wenyi et al. used 2,4,6-trihydroxyacetophenone as the starting material to fully synthesize genkwain. This method has many impurities, and the resulting product has low purity and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take genkwa herb and crush it through a 40-mesh sieve, put 1kg into a microwave extraction tank, add 8L of 60% ethanol solution, extract for 1 hour, extract the extract, then add 6L of 60% ethanol for extraction for 20 minutes, combine the extracts and concentrate under reduced pressure to No alcohol smell, add an equal volume of diethyl ether to extract 3 times, discard the diethyl ether layer to obtain the water layer; adjust the concentration of the water layer to 0.4g / ml, add HPD600 macroporous adsorption resin for adsorption, the sample loading flow rate is 2BV / h, using The diameter-to-height ratio of the column is 1:4, and it is eluted with 30%, 60%, and 90% ethanol in sequence, and the eluted part of 90% ethanol is collected, concentrated under reduced pressure to obtain 36 g of concentrate, and cyclohexane, ethyl acetate, methanol, Water is mixed according to the volume ratio of 10:10:6:3, placed in a separatory funnel for stratification, the upper phase is taken...

Embodiment 2

[0018] Take genkwa herb and crush it through a 40-mesh sieve, put 1kg into a microwave extraction tank, add 6L of 70% ethanol solution, extract for 1 hour, extract the extract, then add 6L of 70% ethanol for extraction for 30 minutes, extract the extract, and then add Extract with 4L of 70% ethanol for 20 minutes, concentrate the combined extracts under reduced pressure until there is no alcohol smell, add an equal volume of ether to extract 5 times, discard the ether layer, and obtain the water layer; adjust the concentration of the water layer to 0.6g / ml, add HPD600 Pore ​​adsorption resin adsorption, the flow rate of sample loading is 1BV / h, the ratio of column diameter to height is 1:6, eluted with 30%, 60%, and 90% ethanol in sequence, and the eluted part of 90% ethanol is collected, concentrated under reduced pressure to obtain concentrated Mix 34g of cyclohexane, ethyl acetate, methanol, and water in a volume ratio of 8:11:3:5, place layers in a separatory funnel, take t...

Embodiment 3

[0020] Take genkwa herb and crush it through a 40-mesh sieve, put 1kg into a microwave extraction tank, add 10L of 85% ethanol solution, extract for 1.5 hours, extract the extract, then add 5L of 85% ethanol for extraction for 50 minutes, extract the extract, and then add 3L of 85% ethanol, the combined extracts were concentrated under reduced pressure until there was no alcohol smell, added an equal volume of ether for extraction 3 times, discarded the ether layer, and obtained the water layer; adjusted the concentration of the water layer to 0.5g / ml, added AB-8 macroporous Adsorbed by adsorption resin, the flow rate of sample loading is 2BV / h, the ratio of column diameter to height is 1:3, eluted with 30%, 60%, and 90% ethanol in sequence, the eluted part of 90% ethanol is collected, and concentrated under reduced pressure to obtain a concentrate 29g, mix cyclohexane, ethyl acetate, methanol, and water at a volume ratio of 12:9:4:4, place layers in a separatory funnel, take t...

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Abstract

The invention provides a method for extracting genkwanin from Daphne genkwa Daphne genkwa Sieb.et Zucc. The method comprises the following steps: smashing raw material Daphne genkwa Sieb.et Zucc., and then adding 60-85% ethanol solution for microwave-assisted extraction; concentrating extract; extracting for multiple times with diethyl ether; abandoning a diethyl ether layer; adding macroporous resin in a water layer for absorption; carrying out gradient elution with water-alcohol; concentrating eluent so as to obtain concentrate; separating and purifying with a high-speed counter-current chromatography, wherein cyclohexane-ethyl acetate-methanol-water is used as a solvent system; concentrating and drying a separated liquid; and recrystallizing with cyclohexane-acetone so as to obtain the product. The genkwanin obtained by using the method has high purity, large preparation amount and low cost, and is an environmentally-friendly purification method.

Description

Technical field: [0001] The invention relates to a method for extracting genkwain from Daphne genkwa, in particular to a method for extracting and purifying genkwain by using a macroporous adsorption resin and high-speed countercurrent chromatography. Background technique: [0002] Genkwanin is also known as genkwanin, and its chemical name is 4', 5-dihydroxy-7-methoxyflavone. Molecular formula C 16 h 12 o 5 , molecular weight 284.26, yellow needle crystal (methanol), mp.286°C. It has various biological activities such as anti-inflammation, anti-oxidation, anti-aging, anti-tumor, anti-mutagenesis, etc. It is widely used in industries such as cosmetics, medicine, and food. Yang Xiaofeng and others have studied it as an ideal non-toxic Pollution pesticides are friendly to the environment, people and animals. [0003] Daphne genkwa is the dried flower bud of Daphne genkwa Sieb.et Zucc., which is recorded in the 2010 edition of the Chinese Pharmacopoeia (Part One). It is bi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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