New method for purifying nettle extract 3,4-divanilyltetrahydrofuran

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

Active Publication Date: 2014-11-19
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 divanillyl tetrahydrofuran in nettles by using ultra-high pressure extraction and column chromatography coupling technology. The steps are as follows:

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

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

[0015] (3) With a flow rate of 2BV / h, carry out gradient elution with ethyl acetate-methanol under the conditions of 3:1, 4:1, and 5:1, track and monitor by thin-layer chromatog...

Embodiment example 2

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

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

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

[0022] (3) With a flow rate of 3BV / h, carry out gradient elution with ethyl acetate-methanol under the condition of 3-5:1, track and monitor by thin-layer chromatography, and collect the fraction containing 3,4 divanillyl tetra...

Embodiment example 3

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

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

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

[0029] (3) at a flow rate of 3BV / h, use petroleum ether-ethanol to carry out gradient elution under the condition of 3-5:1, track and monitor by thin-layer chromatography, and collect the fraction containing 3,4 divanillyl tet...

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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, in particular to a method for significantly increasing 3,4 divanillyl tetrahydrofuran in nettle by using ultra-high pressure extraction and column chromatography coupling technology. Methods for the purity of tetrahydrofuran. Background technique: [0002] Stinging nettle: alias stinging grass, biting grass, scorpion grass, anti-theft grass, ruthless grass, plant cat, biting cat, is a perennial herb of the family Urticaceae, with opposite leaves, monoecious or dioecious, The stinging hairs on its stems and leaves are toxic (anaphylaxis), and its toxicity causes irritant dermatitis immediately after skin contact. The whole herb of nettle can be used as medicine. It tastes bitter, pungent, warm in nature and slightly poisonous. It has the effects of dispelling wind, calming convulsions, eliminating food and laxative. ...

Claims

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Application Information

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Patent Type & Authority Patents(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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