CN102584766A - Method for simultaneously separating dihydromyricetin and myricetin from ampelopsis plant - Google Patents
Method for simultaneously separating dihydromyricetin and myricetin from ampelopsis plant Download PDFInfo
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- CN102584766A CN102584766A CN2011104583477A CN201110458347A CN102584766A CN 102584766 A CN102584766 A CN 102584766A CN 2011104583477 A CN2011104583477 A CN 2011104583477A CN 201110458347 A CN201110458347 A CN 201110458347A CN 102584766 A CN102584766 A CN 102584766A
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- ampelopsin
- dibydro myricetrin
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- myricetin
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Abstract
The invention discloses a method for simultaneously separating dihydromyricetin and myricetin from an ampelopsis plant. The method comprises the following steps of: drying a sample, roughly smashing to 20-40 meshes, extracting with boiling water twice, combining extracting solutions, performing suction filtration in a hot state, standing a filtrate at the temperature of 0-4 DEG C for separating a white precipitate out, performing suction filtration or centrifuging, dissolving the filtrated precipitate with absolute ethyl alcohol, standing, performing suction filtration, concentrating a filtrate under reduced pressure to obtain a thick solution, evaporating ethanol to dryness, and drying at a controlled temperature to obtain general flavone; performing reflux extraction on the general flavone with acetone, concentrating an extracting solution to obtain crude dihydromyricetin, performing reflux extraction on insoluble residues by using ethanol and water in the ratio of 1:1, and concentrating an extracting solution to obtain crude myricetin 1; and during recrystallization and purification of dihydromyricetin with water (recrystallization times are more than three), filtering by heating (to 85-95 DEG C) to obtain a yellow transparent solution serving as a filtrate, collecting a large quantity of yellow green substances (myricetin 2) on filter paper, and drying to obtain myricetin 2. According to HPLC (High Performance Liquid Chromatography) detection, the purity of myricetin 2 is 87.37 percent, and the purity of dihydromyricetin (while needle crystal) is 89.87 percent.
Description
Technical field
The present invention relates to Vitaceae ampelopsis chemical ingredients extraction and separation technology field, can be used for separating when ampelopsin is with dibydro myricetrin in ampelopsis cauline leaf and the processed goods vine tea thereof.
Background technology
All contain flavone component ampelopsin and dibydro myricetrin in the plant of Vitaceae Ampelopsis, wherein with Ampelopsis grossedentata (
Ampelopsis-grossedentada) content is the highest, the processed goods of Ampelopsis grossedentata cauline leaf is commonly called as vine tea, vine tea has multiple physiologically active, main effective constituent is flavonoid compound, and with the dihydromyricetin cellulose content for the highest, the main active ingredient flavones content can be up to more than 40%.In addition, also contain multiple compositions such as ampelopsin, catechin, gallic acid, amino acid, trace element; The staple dibydro myricetrin and the ampelopsin of vine tea flavone, U.S. FDA is widely used in medicine, food, healthcare products and makeup with ampelopsin; And dibydro myricetrin has multiple efficacies such as removing radical, anti-oxidant, antithrombotic, antitumor, anti-inflammatory, is widely used in treating respiratory tract infection, crapulent Chinese patent medicine preparation and has obtained patent of invention in the Application Areas of preparation leukemia and medicine for nasopharyngeal; Be liver protecting, the non-defective unit of Dealcoholic sobering-up can be used as the medical material medicine.But because dibydro myricetrin and ampelopsin all belong to poly-hydroxy flavonols compound; Structure and physico-chemical property are close; And ampelopsin and the dibydro myricetrin content difference in the vine tea of Guizhou is bigger; Ampelopsin content is 1 ~ 3%, and the dihydromyricetin cellulose content can reach 18 ~ 25%, so the high efficiency separation of ampelopsin and dibydro myricetrin composition is to hinder it to be applied to the technical barrier of industrial sectorization in the vine tea always.According to present document and patent report; Adopt classical extraction and separation method such as ethanol refluxing process; Mostly decocting method etc. is single the higher dibydro myricetrin of content is carried out separation and purification, has proposed to vine tea cured leaf solvent soaking wet vine tea leaf microwave radiation processing like Chinese patent-a kind of method (patent No. 200510032918.5) of from vine tea, extracting dibydro myricetrin; Heating in water bath extracts, and uses the method for cold water recrystallization separation and purification dibydro myricetrin then.This method is simple to operate, and impurity is few, and cost is low, but can not separate ampelopsin simultaneously.The separation purification method efficiently that relates to dibydro myricetrin or ampelopsin has at present then cooperated stripping technique in various modern age, mainly is various chromatographic techniques.The document of delivering mainly contains: " separation of ampelopsin and structure are identified in Yao nationality's vine tea " of Chinese national medicine magazine; " the utilizing dibydro myricetrin and ampelopsin in the high-speed countercurrent chromatography while purifying vine tea " of " modern chemical industry "; " heat dissolving, be incubated post, the warm water desorb " of " natural product exploitation " obtained through refining dibydro myricetrin () "; " ampelopsin and dibydro myricetrin separates and the anti-myocardial apoptosis effect in the vine tea " of " Harbin Medical University's journal ".This type of technology mainly is to adopt water to carry or alcohol extracting method; Microwave or ultrasonic auxiliary extraction technology obtain high-load total flavones in addition; Cooperate various chromatographic techniques such as silica gel column chromatography then, polyamide column chromatography, macroporous resin adsorption chromatogram; High speed adverse current chromatograms etc. adopt suitable flow phase system to separate with suitable operational condition according to the purpose needs and obtain ampelopsin or dibydro myricetrin.This class methods separation efficiency is high, and purity is high, but the investment on producing of this method is big, and preparative-scale is little, and operational requirement is high, is unfavorable for suitability for industrialized production.Domestic also have adopting solvent-extraction process to separate the report of ampelopsin and dibydro myricetrin simultaneously." Study on extraction of flavones ingredient in the vine tea of Guangxi " of " contemporary Chinese application pharmacy " proposes; Utilize ampelopsin and the dibydro myricetrin solvability difference in acetone; Can the flavones bullion that extraction obtains be used the acetone refluxing extraction, extracting solution concentrates back water recrystallization and obtains dibydro myricetrin, and insoluble sludge extracts with ethanol-water mixed solvent again; Concentrate, can get the ampelopsin crystallization after leaving standstill a few days.Though this method is simple and easy to operate, it is impure more to extract the ampelopsin that obtains, and pick-up rate is low.Consult domestic and foreign literature, do not see as yet so far and a kind ofly can efficiently separate ampelopsin and dibydro myricetrin simultaneously, and can be expected to apply to the separation method of suitability for industrialized production with the simple solvent method.
Summary of the invention
The present invention separates difficulty in order to solve ampelopsin with dibydro myricetrin, and is difficult to apply to industrialized problem, a kind of method of from ampelopsis, separating dibydro myricetrin and ampelopsin simultaneously of special proposition.
The objective of the invention is to realize through following technical proposals.The method of 1, from ampelopsis, separating dibydro myricetrin and ampelopsin simultaneously; Comprise (1) step that water extracting alcohol dissolves refined total flavonoids from ampelopsis coarse crushing sample; The step of (2) just separating dibydro myricetrin with acetone refluxing extraction total flavones; (3) extract the step that insoluble sludge separates ampelopsin with alcohol-water, the step of water recrystallization purifying dibydro myricetrin and ampelopsin is adopted in (4).It is characterized in that when adopting water recrystallization purifying dibydro myricetrin, the ampelopsin that will just separate in the dibydro myricetrin that obtains through the heating and filtering operation separates with dibydro myricetrin.
2. method of separating ampelopsin and dibydro myricetrin simultaneously according to claim 1 is characterized in that described alcohol-water extracts the step (3) that insoluble sludge separates ampelopsin, and the ratio of alcohol-water is 1:1.
3. method of separating ampelopsin and dibydro myricetrin simultaneously according to claim 1; The step (4) that it is characterized in that described recrystallization purifying dibydro myricetrin and ampelopsin; The heating and filtering service temperature should be 85-95 ℃, and till filtering solution is heated to be yellow-green colour.
4. method of separating ampelopsin and dibydro myricetrin simultaneously as claimed in claim 1 is characterized in that the step (4) of described recrystallization purifying dibydro myricetrin, and the recrystallization number of times of dibydro myricetrin should >=3 times.
The present invention contrasts in the past, and separation method has following innovative point:
1. obtain ampelopsin through the operation of recrystallization heating and filtering first;
2. can obtain ampelopsin by two approach;
3. adopt solvent method to isolate high purity ampelopsin and dibydro myricetrin simultaneously merely.
The present invention contrasts in the past, and separation method has the following advantages:
1. simple to operate, pollute few;
2. product purity is high, and output is high;
2. equipment is simple, and expense is low, is suitable for suitability for industrialized production.
Embodiment 1
Ampelopsis grossedentata (
Ampelopsis-grossedentada(Hand-Mazz) total flavones extracts with refining W.T.Wang)
Take by weighing dry raw and pulverize Ampelopsis grossedentata cauline leaf sample 100g, boiling water extraction adds water 1000mL for the first time at twice, heated and boiled 5 ~ 10 minutes, and inclining decoction liquor; Add 500 ~ 1000mL water again, heated and boiled 5 ~ 10 minutes, united extraction liquid, suction filtration while hot; Filtrating is left standstill at 0 ℃ ~ 4 ℃ and is separated out white precipitate, suction filtration, and the filter deposition is used the 100mL anhydrous alcohol solution, leaves standstill suction filtration; When filtrate decompression was concentrated into solution and is thick, inclining dense magma, volatilizes ethanol, yellow block (total flavones); 50 ℃ ~ 65 ℃ dryings, the mortar porphyrize is used in dry back, weighs, and pours into then to be used in the paper web separating.
2. dibydro myricetrin separates
Get the total flavones that said extracted obtains, as solvent Suo Shi refluxing extraction, vat liquor no longer occurs till the yellow in refluxing extraction to the paper web with 200mL acetone.When extracting solution was directly gone up the Rotary Evaporators concentrating under reduced pressure and is thick, inclining liquid, puts into stink cupboard, volatilizes acetone, and block is gone in the beaker, adds a certain amount of zero(ppm) water, separated out a large amount of yellow-whites depositions after stirring with glass stick immediately.
3. ampelopsin separates
Get insoluble sludge in the above-mentioned cellulose thimble, 100mL carried out the Suo Shi refluxing extraction 1 ~ 3 hour as solvent with alcohol-water (1:1), 85～95 ℃ of bath temperatures.Mixed solvent extracting solution color is pale brown look.When extracting solution was evaporated to small volume, solution took on a red color.Solution is poured in the Erlenmeyer flask, be put in 0～4 ℃ of environment and leave standstill a few days, separate out the tawny deposition, filter, the deposition kept dry with funnel.
4. recrystallization purifying
A large amount of yellow-white depositions of the adding zero(ppm) water that obtains after separating are used the water-bath heating for dissolving, and bath temperature is at 85～95 ℃.When treating that solution thoroughly is yellow-green colour, suction filtration while hot, filtrating is yellow transparent solution, and a large amount of yellow-green colour materials are arranged on the filter paper, it is collected dry.Filtrating behind the suction filtration is poured in the Erlenmeyer flask, and is labelled, under 0-4 ℃ of temperature, leaves standstill.Solution is separated out white precipitate, is cotton-shaped.To precipitate suction filtration, and discard yellow-green colour filtrating, deposition continues to use the zero(ppm) water recrystallization; Collect yellow-green colour material on the filter paper; Continuation will be filtrated and left standstill crystallization at 0-4 ℃, all obtain white needle when operating in for the third time with the 4th recrystallization like this, and needle is constantly washed with frozen water in the suction filtration operation repeatedly; Kept dry gets dibydro myricetrin then, 60 ~ 65 ℃ of drying temperatures.
The tawny deposition and the yellow-green colour material that obtain in the aforesaid operations are accredited as ampelopsin by thin-layer chromatography, and white needle thin-layer chromatography is accredited as dibydro myricetrin.Carry out content detection through performance liquid chromatography, ampelopsin 1 (tawny deposition) purity that obtains of method is lower thus, and ampelopsin 2 (yellow-green colour material) purity is 87.37%, and dibydro myricetrin (white needle) purity is 92.87%.
Embodiment 2
Caulis seu folium ampelopsis brevipedunculatae in Guangdong (
Amplelopsis cantoniensisPlanch) extraction of dibydro myricetrin and ampelopsin is with refining in
Take by weighing dry raw and pulverize Caulis seu folium ampelopsis brevipedunculatae in Guangdong cauline leaf sample 100g, boiling water extraction adds water 1000mL for the first time at twice, heated and boiled 5 ~ 10 minutes, and inclining decoction liquor; Add 500 ~ 1000mL water again, heated and boiled 5 ~ 10 minutes, united extraction liquid, suction filtration while hot; Filtrating is left standstill at 0 ℃ ~ 4 ℃ and is separated out white precipitate, suction filtration, and the filter deposition is used the 100mL anhydrous alcohol solution, leaves standstill suction filtration; When filtrate decompression was concentrated into solution and is thick, inclining dense magma, volatilizes ethanol, yellow block (total flavones); 50 ℃ ~ 65 ℃ dryings, the mortar porphyrize is used in dry back, weighs, and pours into then to be used in the paper web separating.
2. dibydro myricetrin separates
Get the total flavones that said extracted obtains, as solvent Suo Shi refluxing extraction, vat liquor no longer occurs till the yellow in refluxing extraction to the paper web with 200mL acetone.When extracting solution was directly gone up the Rotary Evaporators concentrating under reduced pressure and is thick, inclining liquid, puts into stink cupboard, volatilizes acetone, and block is gone in the beaker, adds a certain amount of zero(ppm) water, separated out a large amount of yellow-whites depositions after stirring with glass stick immediately.
3. ampelopsin separates
Get insoluble sludge in the above-mentioned cellulose thimble, 100mL carried out the Suo Shi refluxing extraction 1 ~ 2 hour as solvent with alcohol-water (1:1), 85～95 ℃ of bath temperatures.Mixed solvent extracting solution color is pale brown look.When extracting solution was evaporated to small volume, solution took on a red color.Solution is poured in the Erlenmeyer flask, be put in 0～4 ℃ of environment and leave standstill a few days, separate out the tawny deposition, filter with funnel, the deposition kept dry gets ampelopsin.
4. recrystallization purifying
A large amount of yellow-white depositions of the adding zero(ppm) water that obtains after separating are used the water-bath heating for dissolving, and bath temperature is at 85～95 ℃.When treating that solution thoroughly is yellow-green colour, suction filtration while hot, filtrating is yellow transparent solution, and a large amount of yellow-green colour materials are arranged on the filter paper, it is collected dry.Filtrating behind the suction filtration is poured in the Erlenmeyer flask, and is labelled, under 0-4 ℃ of temperature, leaves standstill.Solution is separated out white precipitate, is cotton-shaped.To precipitate suction filtration, and discard yellow-green colour filtrating, deposition continues to use the zero(ppm) water recrystallization; Collect yellow-green colour material on the filter paper; Continuation will be filtrated and left standstill crystallization at 0-4 ℃, all obtain white needle when operating in for the third time with the 4th recrystallization like this, and needle is constantly washed with frozen water in the suction filtration operation repeatedly; Kept dry gets dibydro myricetrin then, 60 ~ 65 ℃ of drying temperatures.
The tawny deposition and the yellow-green colour material that obtain in the aforesaid operations are accredited as ampelopsin by thin-layer chromatography, and white needle thin-layer chromatography is accredited as dibydro myricetrin.Carry out content detection through performance liquid chromatography, ampelopsin 1 (tawny deposition) purity that obtains of method is lower thus, and ampelopsin 2 (yellow-green colour material) purity is 85.3%, and dibydro myricetrin (white needle) purity is 90.1%.
Claims (6)
1. a method of from the ampelopsis cauline leaf, separating ampelopsin and dibydro myricetrin simultaneously comprises the steps: the coarse crushing of (1) ampelopsis cauline leaf, and water extracting alcohol dissolves the step of refined total flavonoids; The step of (2) just separating dibydro myricetrin with acetone refluxing extraction total flavones; (3) extract the step that insoluble sludge separates ampelopsin with alcohol-water; (4) step of employing water recrystallization purifying dibydro myricetrin and ampelopsin.
2. it is characterized in that when adopting water recrystallization purifying dibydro myricetrin, the ampelopsin that will just separate in the dibydro myricetrin that obtains through the heating and filtering operation separates with dibydro myricetrin.
3. method of separating ampelopsin and dibydro myricetrin simultaneously according to claim 1 is characterized in that described alcohol-water extracts the step (3) that insoluble sludge separates ampelopsin, and the ratio of alcohol-water is 1:1.
4. method of separating ampelopsin and dibydro myricetrin simultaneously according to claim 1; The step (4) that it is characterized in that described recrystallization purifying dibydro myricetrin and ampelopsin; The heating and filtering service temperature should be 85-95 ℃, and till filtering solution is heated to be yellow-green colour.
5. method of separating ampelopsin and dibydro myricetrin simultaneously as claimed in claim 1 is characterized in that the step (4) of described recrystallization purifying dibydro myricetrin, and the recrystallization number of times of dibydro myricetrin should >=3 times.
6. the inventive method is not only applicable to separating of ampelopsin and dibydro myricetrin in the ampelopsis, all is suitable for for other platymiscium that contains ampelopsin and dibydro myricetrin composition.
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Cited By (8)
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| CN102875510A (en) * | 2012-10-22 | 2013-01-16 | 长沙盛凯生物科技有限公司 | Process method for extracting high-content dihydromyricetin from ampelopsis grossedentata |
| CN103275049A (en) * | 2013-05-21 | 2013-09-04 | 中南大学 | Method for preparing myricetin by using vine tea and application of pyrosulfite |
| EP2762137A1 (en) | 2013-02-05 | 2014-08-06 | Jilinsheng Jinziyuan Biotechnology Ltd. | Use of myricetin or derivatives thereof as a cathepsin k inhibitor |
| CN105037310A (en) * | 2015-06-05 | 2015-11-11 | 柳州市绿翔生物技术有限公司 | Process for simultaneously extracting myricetin and dihydromyricetin |
| CN106008438A (en) * | 2014-12-01 | 2016-10-12 | 华中科技大学同济医学院附属同济医院 | Racemic dihydromyricetin anhydrous substance crystal |
| JP2017178935A (en) * | 2016-03-29 | 2017-10-05 | 株式会社ファンケル | Chymase inhibitory composition |
| CN107892679A (en) * | 2017-11-24 | 2018-04-10 | 贵州大学 | A kind of method of the separating and purifying high-purity dihydromyricetin from ampelopsis |
| CN111892566A (en) * | 2019-05-05 | 2020-11-06 | 首都医科大学 | Ampelopsis grossedentata water extract, preparation method thereof and application of water extract as acetylcholinesterase inhibitor |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875510A (en) * | 2012-10-22 | 2013-01-16 | 长沙盛凯生物科技有限公司 | Process method for extracting high-content dihydromyricetin from ampelopsis grossedentata |
| EP2762137A1 (en) | 2013-02-05 | 2014-08-06 | Jilinsheng Jinziyuan Biotechnology Ltd. | Use of myricetin or derivatives thereof as a cathepsin k inhibitor |
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| CN103275049A (en) * | 2013-05-21 | 2013-09-04 | 中南大学 | Method for preparing myricetin by using vine tea and application of pyrosulfite |
| CN106008438A (en) * | 2014-12-01 | 2016-10-12 | 华中科技大学同济医学院附属同济医院 | Racemic dihydromyricetin anhydrous substance crystal |
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| CN105037310A (en) * | 2015-06-05 | 2015-11-11 | 柳州市绿翔生物技术有限公司 | Process for simultaneously extracting myricetin and dihydromyricetin |
| JP2017178935A (en) * | 2016-03-29 | 2017-10-05 | 株式会社ファンケル | Chymase inhibitory composition |
| CN107892679A (en) * | 2017-11-24 | 2018-04-10 | 贵州大学 | A kind of method of the separating and purifying high-purity dihydromyricetin from ampelopsis |
| CN111892566A (en) * | 2019-05-05 | 2020-11-06 | 首都医科大学 | Ampelopsis grossedentata water extract, preparation method thereof and application of water extract as acetylcholinesterase inhibitor |
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Inventor after: Yu Jianping Inventor after: Yu Jiansheng Inventor after: Yu Haoxiang Inventor after: He Hui Inventor after: Wu Guixiang Inventor after: Fan Jingjing Inventor after: Fan Jiayou Inventor before: Yu Jianping Inventor before: Wu Guixiang Inventor before: Fan Jiayou Inventor before: Yu Haoxiang Inventor before: Fan Jingjing |
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