New method for purifying nettle extract 3,4-divanilyltetrahydrofuran

A technology of tetrahydrofuran and two vanilla, applied in 3 fields, can solve problems such as low extraction purity and low extraction rate

Active Publication Date: 2012-10-17
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of conventional techniques such as relatively low extraction rate and low extraction purity, and provide a method for significantly improving the purity of 3,4 divanillyl tetrahydrofuran in nettles by utilizing ultra-high pressure extraction and column chromatography coupling technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: A method for significantly improving the purity of 3,4-divanillyltetrahydrofuran in nettle using ultra-high pressure extraction and column chromatography coupling technology. The steps are as follows:

[0013] (1) Put the cut sections of dried nettle into a pressure-resistant bag, add 6 times the volume of ethanol with a concentration of 70%, treat it under ultra-high pressure 200MPA, 10min, 20℃, recover the ethanol, and dry it under vacuum at 60℃. Crude:

[0014] (2) Dissolve the obtained crude powder of 3,4 divanillyl tetrahydrofuran in ethyl acetate, add an appropriate amount of pre-activated silica gel, stir, dry the ethyl acetate, pass through a 60 mesh sieve, and apply 200 mesh silica gel column chromatography to an industrial-grade column ;

[0015] (3) At a flow rate of 2BV / h, gradient elution was carried out with ethyl acetate-methanol under 3:1, 4:1, 5:1 conditions, followed by thin layer chromatography, and collected 3,4 divanillyltetrahydrofuran Ingr...

Embodiment example 2

[0019] Implementation case 2: A method for enriching and purifying 3,4 divanillyl tetrahydrofuran in nettle using macroporous adsorption resin, the steps are as follows:

[0020] (1) Put the cut sections of dried nettle into a pressure-resistant bag, add 7 times the volume of ethanol with a concentration of 75%, treat it under ultra-high pressure 300MPA, 15min, 20℃, recover the ethanol, and dry it under vacuum at 60℃. Crude;

[0021] (2) Dissolve the obtained 3,4 divanillyl tetrahydrofuran coarse crystalline powder in ethyl acetate, add an appropriate amount of pre-activated silica gel, stir, dry the ethyl acetate, pass through a 60-mesh sieve, and apply a 300-mesh silica gel column to an industrial-grade column Analyze

[0022] (3) Perform gradient elution with ethyl acetate-methanol under the conditions of 3-5:1 at a flow rate of 3BV / h, followed by thin-layer chromatography, and collect the fraction containing 3,4-divanillyltetrahydrofuran;

[0023] (4) Use a thin layer to determi...

Embodiment example 3

[0026] Implementation case 3: A method for enriching and purifying 3,4 divanillyl tetrahydrofuran in nettle using macroporous adsorption resin, the steps are as follows:

[0027] (1) Put the cut sections of dried nettle into a pressure-resistant bag, add 8 times the volume of ethanol with a concentration of 80%, treat it under ultra-high pressure 400MPA, 12min, 20℃, recover the ethanol, and dry it under vacuum at 60℃. Crude;

[0028] (2) Dissolve the obtained crude powder of 3,4 divanillyl tetrahydrofuran in ethyl acetate, add an appropriate amount of pre-activated silica gel, stir, dry the ethyl acetate, pass through a 60 mesh sieve, and apply 200 mesh silica gel column chromatography to an industrial-grade column ;

[0029] (3) At a flow rate of 3BV / h, use petroleum ether-ethanol to perform gradient elution under the conditions of 3-5:1, followed by thin-layer chromatography, and collect the 3,4-divanillyltetrahydrofuran fraction;

[0030] (4) Use a thin layer to determine the 3,4...

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PUM

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Abstract

The present invention belongs to the field of natural organic chemistry, relates to a method for purifying 3,4-divanilyltetrahydrofuran, and especially to a method for substantially improving purity of 3,4-divanilyltetrahydrofuran in nettle by using a super-pressure extraction and column chromatography combined technology. The method has the following advantages that: 1, the super-pressure technology adopts normal temperature and near normal temperature conditions, and the solvent can enter the plant cell interior with the super-pressure so as to provide the high extraction efficiency for active ingredients without destruction of biological active ingredients; 2, the silica gel column chromatography is adopted, such that the separation effect is good, and the product purity is high; and 3, no solvent is remained during the extraction process, such that the product safety is high. With the present invention, the super-pressure extraction and column chromatography combined technology is adopted, ethanol is firstly adopted as the solvent, the super-pressure extraction with static pressure more than 100 is performed, the active ingredients can overflow along with the solvent after the pressure is released, silica gel column chromatography separation is performed, and recrystallization is performed to obtain the purified 3,4-divanilyltetrahydrofuran, wherein the purity of the 3,4-divanilyltetrahydrofuran in the nettle is increased to 98%.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for purifying 3,4 divanillyl tetrahydrofuran, and in particular to a method using ultra-high pressure extraction and column chromatography coupling technology to significantly improve the 3,4 divanillyl tetrahydrofuran in nettle Method for purity of tetrahydrofuran. Background technique: [0002] Nettle: also known as stinging grass, biting grass, scorpion grass, anti-theft grass, ruthless grass, plant cat, biting cat, it is a perennial herb of the genus Urtica in the family Urtica, with opposite leaves, monoecious or different, The sting hairs on its stems and leaves are toxic (allergic reaction), and its toxicity can cause irritant dermatitis immediately after skin contact. The whole nettle herb can be used as medicine. Its taste is bitter, pungent, warm in nature, and slightly poisonous. It has the effects of dispelling wind, calming convulsions, and eliminating f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/12
Inventor 姚德坤姚德利张亚红万莉
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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