CN109369595A - A method of dihydromyricetin is extracted from ampelopsis grossdentata - Google Patents

A method of dihydromyricetin is extracted from ampelopsis grossdentata Download PDF

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Publication number
CN109369595A
CN109369595A CN201811206590.8A CN201811206590A CN109369595A CN 109369595 A CN109369595 A CN 109369595A CN 201811206590 A CN201811206590 A CN 201811206590A CN 109369595 A CN109369595 A CN 109369595A
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China
Prior art keywords
ampelopsis grossdentata
solution
added
value
dihydromyricetin
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CN201811206590.8A
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尹婷
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CHANGSHA SHENGKAI BIOLOGICAL TECHNOLOGY Co Ltd
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CHANGSHA SHENGKAI BIOLOGICAL TECHNOLOGY Co Ltd
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Priority to CN201811206590.8A priority Critical patent/CN109369595A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/28Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
    • C07D311/322,3-Dihydro derivatives, e.g. flavanones
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/40Separation, e.g. from natural material; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of methods for extracting dihydromyricetin from ampelopsis grossdentata, comprising the following steps: (1) pre-processes;(2) it digests;(3) it extracts;(4) it is concentrated;(5) primary crystal;(6) it recrystallizes;(7) it purifies;(8) it is dried in vacuo.The present invention can improve the yield and purity of dihydromyricetin.

Description

A method of dihydromyricetin is extracted from ampelopsis grossdentata
Technical field
The present invention relates to the extracting methods of dihydromyricetin, in particular to a kind of to extract dihydromyricetin from ampelopsis grossdentata Method.
Background technique
Ampelopsis grossdentata alias vine tea, Maoyanmei tea are a kind of wild bejucoes, and wherein main active is Dihydromyricetin.Dihydromyricetin, which has, removes a variety of peculiar effects such as free radical, anti-oxidant, antithrombotic, antitumor, anti-inflammatory; And dihydromyricetin is a kind of more special flavone compound, is releasing alcoholism, prevention alcoholic liver, fatty liver, inhibition Disease incidence, the anti-hypertension, the formation for inhibiting extracorporeal platelet aggregation and internal thrombus, reduction that liver cell deteriorates, reduces liver cancer Blood lipid and blood glucose level, improving superoxide dismutase activity and liver protecting etc. has special efficacy.And it is existing The yield of dihydromyricetin extractive technique is not high, and the purity of resulting dihydromyricetin is also to be improved.
Summary of the invention
The purpose of the present invention is making improvement and innovation for shortcoming and defect present in background technique, provide it is a kind of from The method that ampelopsis grossdentata extracts dihydromyricetin, this method can improve the yield and purity of dihydromyricetin.
To achieve the above object, the technical solution adopted by the present invention is that: it is a kind of to extract dihydromyricetin from ampelopsis grossdentata Method, comprising the following steps:
(1) it pre-processes: fresh ampelopsis grossdentata leaf being toasted, then takes out and is ground into 20 mesh particles, ampelopsis grossdentata is made Ye Fen;
(2) it digests: ampelopsis grossdentata leaf powder being mixed with deionized water, and complex enzyme is added and stirs evenly, place 1 ~ 2h, be made Enzymolysis liquid;
(3) it extracts: enzymolysis liquid is filtered with centrifuge, obtain aqueous solution, filtered solid is put into the hot second that concentration is 90% In alcoholic solution, 1h is handled with ultrasonic extraction tank, then filters pressing obtains ethanol solution, and aqueous solution and ethanol solution are mixed to prepare Stoste;
(4) it is concentrated: stoste being concentrated into 0.5 times of amount of raw material weight, concentrate is made;
(5) primary crystal: adjusting the pH value of concentrate with hydrochloric acid, stand under cryogenic, precipitating is collected by filtration, and crude product is made;
(6) recrystallize: by crude product be added boiling water dissolution, and use the pH value of hydrochloric acid conditioning solution, stand under cryogenic, filtering Precipitating is collected, is repeated twice, semi-finished product are made;
(7) it purifies: the ethanol solution that concentration is 90% is added in semi-finished product and is dissolved, and with the pH value of hydrochloric acid conditioning solution, low It is stood under the conditions of temperature, precipitating, finished product is collected by filtration;
(8) it is dried in vacuo: placing products into dry 14 ~ 16h in vacuum oven.
Preferably, the temperature of baking described in step (1) is 90 ~ 100 DEG C, and baking time is 3 ~ 4h.
Preferably, deionized water temperature described in step (2) is 40 ~ 50 DEG C, the weight Zhan Xianchi snake Portugal of the complex enzyme The 2% ~ 3% of grape leaf powder weight.
Preferably, salt acid for adjusting pH value is added to 4 ~ 5 in concentrate described in step (5), stands for 24 hours at 5 ~ 8 DEG C.
Preferably, salt acid for adjusting pH value is added to 4 ~ 5 in solution described in step (6) and (7), stands 12h at 5 ~ 8 DEG C. Advantages of the present invention and the utility model has the advantages that
The present invention uses fresh ampelopsis grossdentata leaf, and by high-temperature baking, the method dried in the shade compared to tradition can be protected preferably Dihydromyricetin is stayed, dihydromyricetin is avoided to lose, while the present invention cracks the cell wall of ampelopsis grossdentata leaf using complex enzyme, Make intracellular substance release, improves the yield of dihydromyricetin.The present invention is assisted from enzymatic hydrolysis residue using ultrasonic wave Dihydromyricetin is extracted, the special work such as judder, high acceleration, strong cavitation effect, stirring generated by ultrasonic wave With, promote ethyl alcohol dissolve dihydromyricetin, to greatest extent improve dihydromyricetin yield.The present invention is adjusted molten using hydrochloric acid The pH value of liquid greatly reduces the solubility of dihydromyricetin, while crystallizing in cryogenic conditions, improves crystalline rate to 4 ~ 5 And yield.The present invention is recrystallized to give higher degree first with deionized water using the method for recrystallization and different solvents crystallization Dihydromyricetin, recycle 90% ethanol solution crystallizing to purify to obtain the dihydromyricetin of high-purity, purifying technique is simple, It is low in cost, substantially increase the purity of dihydromyricetin.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Embodiment 1
A method of dihydromyricetin is extracted from ampelopsis grossdentata, comprising the following steps:
(1) it pre-processes: fresh ampelopsis grossdentata leaf being toasted into 3h at a temperature of 90 DEG C, then takes out and is ground into 20 mesh particles, Ampelopsis grossdentata leaf powder is made.
(2) it digests: ampelopsis grossdentata leaf powder is mixed with 40 DEG C of deionized water, and be added and account for the compound of leaf powder weight 2% Enzyme stirs evenly, and places 1h, and enzymolysis liquid is made.
(3) it extracts: enzymolysis liquid is filtered with centrifuge, obtain aqueous solution, it is 90% that filtered solid, which is put into concentration, In hot ethanol solution, 1h is handled with ultrasonic extraction tank, then filters pressing obtains ethanol solution, and aqueous solution is mixed with ethanol solution Stoste is made.
(4) it is concentrated: stoste being concentrated into 0.5 times of amount of raw material weight, concentrate is made.
(5) primary crystal: the pH value for adjusting concentrate with hydrochloric acid stands for 24 hours at 5 DEG C to 4, precipitating is collected by filtration, be made Crude product.
(6) it recrystallizes: boiling water dissolution is added in crude product, and with the pH value of hydrochloric acid conditioning solution to 4, is stood at 5 DEG C 12h is collected by filtration precipitating, is repeated twice, and semi-finished product are made.
(7) it purifies: the ethanol solution that concentration is 90% is added in semi-finished product and is dissolved, and extremely with the pH value of hydrochloric acid conditioning solution 4,12h is stood at 5 DEG C, and precipitating, finished product is collected by filtration.
(8) it is dried in vacuo: placing products into dry 14h in vacuum oven.
Embodiment 2
A method of dihydromyricetin is extracted from ampelopsis grossdentata, comprising the following steps:
(1) it pre-processes: fresh ampelopsis grossdentata leaf being toasted into 3h at a temperature of 95 DEG C, then takes out and is ground into 20 mesh particles, Ampelopsis grossdentata leaf powder is made.
(2) it digests: ampelopsis grossdentata leaf powder is mixed with 45 DEG C of deionized water, and be added and account for answering for leaf powder weight 2.5% Synthase stirs evenly, and places 1.5h, and enzymolysis liquid is made.
(3) it extracts: enzymolysis liquid is filtered with centrifuge, obtain aqueous solution, it is 90% that filtered solid, which is put into concentration, In hot ethanol solution, 1h is handled with ultrasonic extraction tank, then filters pressing obtains ethanol solution, and aqueous solution is mixed with ethanol solution Stoste is made.
(4) it is concentrated: stoste being concentrated into 0.5 times of amount of raw material weight, concentrate is made.
(5) primary crystal: the pH value for adjusting concentrate with hydrochloric acid stands for 24 hours at 6 DEG C to 4, precipitating is collected by filtration, be made Crude product.
(6) it recrystallizes: boiling water dissolution is added in crude product, and with the pH value of hydrochloric acid conditioning solution to 4, is stood at 6 DEG C 12h is collected by filtration precipitating, is repeated twice, and semi-finished product are made.
(7) it purifies: the ethanol solution that concentration is 90% is added in semi-finished product and is dissolved, and extremely with the pH value of hydrochloric acid conditioning solution 4,12h is stood at 6 DEG C, precipitating, finished product is collected by filtration.
(8) it is dried in vacuo: placing products into dry 15h in vacuum oven.
Embodiment 3
A method of dihydromyricetin is extracted from ampelopsis grossdentata, comprising the following steps:
(1) it pre-processes: fresh ampelopsis grossdentata leaf being toasted into 4h at a temperature of 100 DEG C, then takes out and is ground into 20 mesh particles, Ampelopsis grossdentata leaf powder is made.
(2) it digests: ampelopsis grossdentata leaf powder is mixed with 50 DEG C of deionized water, and be added and account for the compound of leaf powder weight 3% Enzyme stirs evenly, and places 2h, and enzymolysis liquid is made.
(3) it extracts: enzymolysis liquid is filtered with centrifuge, obtain aqueous solution, it is 90% that filtered solid, which is put into concentration, In hot ethanol solution, 1h is handled with ultrasonic extraction tank, then filters pressing obtains ethanol solution, and aqueous solution is mixed with ethanol solution Stoste is made.
(4) it is concentrated: stoste being concentrated into 0.5 times of amount of raw material weight, concentrate is made.
(5) primary crystal: the pH value for adjusting concentrate with hydrochloric acid stands for 24 hours at 8 DEG C to 5, precipitating is collected by filtration, be made Crude product.
(6) it recrystallizes: boiling water dissolution is added in crude product, and with the pH value of hydrochloric acid conditioning solution to 5, is stood at 8 DEG C 12h is collected by filtration precipitating, is repeated twice, and semi-finished product are made.
(7) it purifies: the ethanol solution that concentration is 90% is added in semi-finished product and is dissolved, and extremely with the pH value of hydrochloric acid conditioning solution 5,12h is stood at 8 DEG C, precipitating, finished product is collected by filtration.
(8) it is dried in vacuo: placing products into dry 16h in vacuum oven.
The technical principle of the invention is described above in combination with a specific embodiment.These descriptions are intended merely to explain of the invention Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, the technology of this field Personnel can associate with other specific embodiments of the invention without creative labor, these modes are fallen within Within protection scope of the present invention.

Claims (5)

1. a kind of method for extracting dihydromyricetin from ampelopsis grossdentata, it is characterised in that following steps:
(1) it pre-processes: fresh ampelopsis grossdentata leaf being toasted, then takes out and is ground into 20 mesh particles, ampelopsis grossdentata is made Ye Fen;
(2) it digests: ampelopsis grossdentata leaf powder being mixed with deionized water, and complex enzyme is added and stirs evenly, place 1 ~ 2h, be made Enzymolysis liquid;
(3) it extracts: enzymolysis liquid is filtered with centrifuge, obtain aqueous solution, filtered solid is put into the hot second that concentration is 90% In alcoholic solution, 1h is handled with ultrasonic extraction tank, then filters pressing obtains ethanol solution, and aqueous solution and ethanol solution are mixed to prepare Stoste;
(4) it is concentrated: stoste being concentrated into 0.5 times of amount of raw material weight, concentrate is made;
(5) primary crystal: adjusting the pH value of concentrate with hydrochloric acid, stand under cryogenic, precipitating is collected by filtration, and crude product is made;
(6) recrystallize: by crude product be added boiling water dissolution, and use the pH value of hydrochloric acid conditioning solution, stand under cryogenic, filtering Precipitating is collected, is repeated twice, semi-finished product are made;
(7) it purifies: the ethanol solution that concentration is 90% is added in semi-finished product and is dissolved, and with the pH value of hydrochloric acid conditioning solution, low It is stood under the conditions of temperature, precipitating, finished product is collected by filtration;
(8) it is dried in vacuo: placing products into dry 14 ~ 16h in vacuum oven.
2. a kind of method according to claim 1, it is characterised in that the temperature of baking described in step (1) is 90 ~ 100 DEG C, baking time is 3 ~ 4h.
3. a kind of method according to claim 1, it is characterised in that deionized water temperature described in step (2) is 40 ~ 50 DEG C, the weight of the complex enzyme accounts for the 2% ~ 3% of ampelopsis grossdentata leaf powder weight.
4. a kind of method according to claim 1, it is characterised in that salt acid for adjusting pH is added in concentrate described in step (5) Value is stood for 24 hours at 5 ~ 8 DEG C to 4 ~ 5.
5. a kind of method according to claim 1, it is characterised in that hydrochloric acid tune is added in solution described in step (6) and (7) PH value is saved to 4 ~ 5, stands 12h at 5 ~ 8 DEG C.
CN201811206590.8A 2018-10-17 2018-10-17 A method of dihydromyricetin is extracted from ampelopsis grossdentata Pending CN109369595A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114532537A (en) * 2022-02-23 2022-05-27 广东农工商职业技术学院 Method for preparing dihydromyricetin nano capsule based on vine tea extract

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105153091A (en) * 2015-08-25 2015-12-16 华中科技大学同济医学院附属同济医院 Method for increasing yield of dihydromyricetin in ampelopsis grossedentata
CN106518829A (en) * 2016-11-10 2017-03-22 张清峰 Method for separating and purifying dihydromyricetin from ampelopsis grossedentata leaves

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105153091A (en) * 2015-08-25 2015-12-16 华中科技大学同济医学院附属同济医院 Method for increasing yield of dihydromyricetin in ampelopsis grossedentata
CN106518829A (en) * 2016-11-10 2017-03-22 张清峰 Method for separating and purifying dihydromyricetin from ampelopsis grossedentata leaves

Non-Patent Citations (2)

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Title
姚茂君等: "二氢杨梅素的超声波辅助溶剂提取工艺", 《食品与生物技术学报》, vol. 26, no. 3, pages 20 - 23 *
陈雁梅: "显齿蛇葡萄制茶废弃茎中二氢杨梅素制备工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 02, pages 018 - 122 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114532537A (en) * 2022-02-23 2022-05-27 广东农工商职业技术学院 Method for preparing dihydromyricetin nano capsule based on vine tea extract

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Application publication date: 20190222