CN110538226A - preparation method for extracting total flavonoids from hovenia dulcis thunb - Google Patents
preparation method for extracting total flavonoids from hovenia dulcis thunb Download PDFInfo
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- CN110538226A CN110538226A CN201810529952.0A CN201810529952A CN110538226A CN 110538226 A CN110538226 A CN 110538226A CN 201810529952 A CN201810529952 A CN 201810529952A CN 110538226 A CN110538226 A CN 110538226A
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- ethanol
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/72—Rhamnaceae (Buckthorn family), e.g. buckthorn, chewstick or umbrella-tree
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses a preparation method for extracting total flavonoids from hovenia dulcis thunb, which is characterized by comprising the following steps of: 1) grinding dried folium Hoveniae into coarse powder; 2) taking the coarse powder, adding 25mL of 75% ethanol, performing reflux extraction for 2 times, each time 80mL, each time for 1-3 h, combining the extracting solutions, and recovering ethanol to obtain hovenia dulcis thunb extract; 3) extraction: adding a proper amount of distilled water into the hovenia dulcis thunb extract, uniformly stirring, adding the mixture into a chromatographic column, adjusting the flow rate to be 5ml/min, washing the mixture with distilled water to remove impurities, and desorbing the mixture by using 10-40% ethanol as a mobile phase; 4) recovering ethanol to obtain total flavone extract, and vacuum drying to obtain total flavone. The total flavone prepared by the method has high product purity, good quality, simple and easy process method, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a preparation method of total flavonoids.
Background
Hovenia acerba is a species of Hovenia of Rhamnaceae. Hovenia dulcis, belonging to Rhamnaceae Hovenia, is a deciduous broad-leaf tall tree with the tree height of up to 30 meters, namely Hovenia dulcis, Crataegus pinnatifida, papaw, sarcocarp, orange twister, Crataegus pinnatifida, and Crataegus pinnatifida, wherein most provinces of China are sporadically distributed and wild. Has medical value, and can clear heat, promote urination, relieve cough, relieve restlessness and relieve alcoholism. Its skin has the functions of promoting blood circulation, relaxing muscles and tendons and detoxicating. Can be used for treating gastrocnemius spasm, food stagnation, and hammer poisoning. The fruit stalks can invigorate the stomach and enrich the blood.
The hovenia dulcis thunb alcohol extract can improve the oxidation function of reduced Glutathione (GSH) of mice with acute liver injury, enhance GSH binding reaction catalyzed by glutathione S-transferase (GST), increase the activities of superoxide dismutase (SOD) and catalase (Cat), and antagonize the mice with acute liver injury caused by ethanol. The 75% ethanol extract of the hovenia dulcis thunb has definite anti-hepatic fibrosis effect. The flavone compounds containing quercetin and the like are separated from hovenia dulcis thunb and possibly are the effective components of the flavone compounds.
the flavonoids generally refer to a series of compounds in which two benzene rings (A-and B-rings) having phenolic hydroxyl groups are connected with each other through a central three-carbon atom, and the basic nucleus of the compounds is 2-phenylchromone. The structure of the flavonoid compound is often connected with functional groups such as phenolic hydroxyl, methoxyl, methyl, isopentenyl and the like. In addition, it is often combined with a sugar to form a glycoside. The total flavonoids compounds in the hovenia dulcis thunb have the obvious functions of resisting oxidation and free radicals, resisting and preventing cancers, lowering blood pressure, regulating blood fat, improving microcirculation, inhibiting bacteria, diminishing inflammation, easing pain and the like.
Disclosure of Invention
the invention aims to provide a method for extracting total flavonoids, and the total flavonoids have wide medicinal and health-care values.
The invention is completed by the following technical scheme, and the specific content comprises the following steps: method for extracting total flavone
1) Grinding dried semen Hoveniae into coarse powder;
2) taking the coarse powder, adding 25mL of 75% ethanol, performing reflux extraction for 2 times, each time 80mL, each time for 1-3 h, combining the extracting solutions, and recovering ethanol to obtain hovenia dulcis thunb extract;
3) Extraction: adding a proper amount of distilled water into the hovenia dulcis thunb extract, uniformly stirring, adding the mixture into a chromatographic column, adjusting the flow rate to be 5ml/min, washing the mixture with distilled water to remove impurities, and desorbing the mixture by using 10-40% ethanol as a mobile phase;
4) Recovering ethanol to obtain total flavone extract, and vacuum drying to obtain total flavone.
The reflux extraction time in the step 2) is 1-3 h.
The chromatographic column in the step 3) is prepared by pretreating D101 type macroporous resin and polyamide, and the content of the mobile phase desorption ethanol is 10-40%.
the invention has the advantages that
The invention adopts ultrasonic extraction-D101 type macroporous resin and polyamide column chromatography to extract the total flavone in the hovenia dulcis thunb, the sample capacity of the column chromatography is large, the extraction efficiency is high, and the method is simple and easy to implement.
the present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.
The specific implementation mode is as follows:
Example 1:
grinding dried semen Hoveniae into coarse powder; adding 75% ethanol 25mL, reflux extracting for 2 times, each time 80mL, each time 1, mixing extractive solutions, and recovering ethanol to obtain semen Hoveniae extract; adding appropriate amount of distilled water into semen Hoveniae extract, stirring, adding into chromatographic column, adjusting flow rate to 5ml/min, washing with distilled water to remove impurities, and desorbing with 10% ethanol as mobile phase; recovering ethanol to obtain total flavone extract, and vacuum drying to obtain total flavone with extraction rate of 87.5%.
Example 2:
Grinding dried semen Hoveniae into coarse powder; adding 75% ethanol 25mL, reflux extracting for 2 times, each time 80mL, each time for 2h, mixing extractive solutions, and recovering ethanol to obtain semen Hoveniae extract; adding appropriate amount of distilled water into semen Hoveniae extract, stirring, adding into chromatographic column, adjusting flow rate to 5ml/min, washing with distilled water to remove impurities, and desorbing with 30% ethanol as mobile phase; recovering ethanol to obtain total flavone extract, and vacuum drying to obtain total flavone with extraction rate of 94.7%.
Example 3:
Grinding dried semen Hoveniae into coarse powder; adding 75% ethanol 25mL, reflux extracting for 2 times, each time 80mL, each time for 3h, mixing extractive solutions, and recovering ethanol to obtain semen Hoveniae extract; adding appropriate amount of distilled water into semen Hoveniae extract, stirring, adding into chromatographic column, adjusting flow rate to 5ml/min, washing with distilled water to remove impurities, and desorbing with 40% ethanol as mobile phase; recovering ethanol to obtain total flavone extract, and vacuum drying to obtain total flavone with extraction rate of 92.1%.
Claims (3)
1. A preparation method for extracting total flavonoids from hovenia dulcis thunb is characterized by comprising the following steps:
1) grinding dried semen Hoveniae into coarse powder;
2) taking the coarse powder, adding 25mL of 75% ethanol, performing reflux extraction for 2 times, each time 80mL, each time for 1-3 h, combining the extracting solutions, and recovering ethanol to obtain hovenia dulcis thunb extract;
3) Extraction: adding a proper amount of distilled water into the hovenia dulcis thunb extract, uniformly stirring, adding the mixture into a chromatographic column, adjusting the flow rate to be 5ml/min, washing the mixture with distilled water to remove impurities, and desorbing the mixture by using 10-40% ethanol as a mobile phase;
4) Recovering ethanol to obtain total flavone extract, and vacuum drying to obtain total flavone.
2. the method for preparing total flavonoids from hovenia dulcis thunb according to claim 1, wherein the reflux extraction time in the step 2) is 1-3 h.
3. The preparation method for extracting total flavonoids from hovenia dulcis thunb according to claim 1, which is characterized in that the chromatographic column in the step 3) is prepared by pretreating D101 type macroporous resin and polyamide, and the content of mobile phase-desorbed ethanol is 10-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810529952.0A CN110538226A (en) | 2018-05-29 | 2018-05-29 | preparation method for extracting total flavonoids from hovenia dulcis thunb |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111603509A (en) * | 2020-06-30 | 2020-09-01 | 河南中大恒源生物科技股份有限公司 | Preparation method of hovenia dulcis thunb extract rich in dihydromyricetin |
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2018
- 2018-05-29 CN CN201810529952.0A patent/CN110538226A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111603509A (en) * | 2020-06-30 | 2020-09-01 | 河南中大恒源生物科技股份有限公司 | Preparation method of hovenia dulcis thunb extract rich in dihydromyricetin |
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Application publication date: 20191206 |