CN104435017A - Extraction method of flavonol in ginkgo leaves - Google Patents

Extraction method of flavonol in ginkgo leaves Download PDF

Info

Publication number
CN104435017A
CN104435017A CN201410631856.9A CN201410631856A CN104435017A CN 104435017 A CN104435017 A CN 104435017A CN 201410631856 A CN201410631856 A CN 201410631856A CN 104435017 A CN104435017 A CN 104435017A
Authority
CN
China
Prior art keywords
folium ginkgo
eluting
extraction
reduced pressure
extraction method
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410631856.9A
Other languages
Chinese (zh)
Inventor
董燕敏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou University
Original Assignee
Changzhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changzhou University filed Critical Changzhou University
Priority to CN201410631856.9A priority Critical patent/CN104435017A/en
Publication of CN104435017A publication Critical patent/CN104435017A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • A61K36/16—Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
    • 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
    • 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
    • A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • 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
    • 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
    • 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
    • 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
    • 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
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

Landscapes

  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to an extraction method of flavonol in ginkgo leaves. The extraction method specifically comprises the following steps: cleaning ginkgo leaves; irradiating by using an ultraviolet lamp; when the gingko leaves wither, drying the gingko leaves in a constant temperature furnace; crushing and sieving; then extracting the gingko leaves in an ethanol solution under the support of ultrasonic waves; and then, filtering the extracted liquid by diatomite, distilling at reduced pressure, extracting by using dichloromethane, purifying, eluting, and finally concentrating at reduced pressure to obtain flavonol. The extraction method provided by the invention is simple and high in extraction rate and effective components are hardly damaged.

Description

The extracting method of flavone in a kind of Folium Ginkgo
Technical field
The present invention relates to a kind of extracting method, particularly the extracting method of flavone in a kind of Folium Ginkgo.
Background technology
Ginkgo is a kind of herba perennis wood species, due to geological changes and climate change, deposits very few at present, also has the title of " living fossil ".Show through domestic and international large quantity research, the effective ingredient extracted from Folium Ginkgo-pyrite compounds, cardiovascular and cerebrovascular disease, senile dementia can be prevented, also have significant curative effect to bronchitis asthma, dermatosis, alopecia, promote blood circulation of human body, brain metabolism, antiinflammatory, antioxidation, regulation of physiological functions in addition.Folium Ginkgo extract can be used for developing nutrient and healthcare products and cosmetics etc. simultaneously, so the research and development of effective component of ginkgo leaf more and more cause the extensive concern of Chinese scholars, Semen Ginkgo persimmon vinegar beverage is exactly wherein a kind of ginkgo health drink, it adds ginkgo biloba succi on persimmon vinegar basis, the allotment such as Mel.
The extracting mode of Flavones from Ginkgo Leaves has decocting in water, supercritical CO 2extraction and organic solvent extractionprocess.Water-boiling method the method has that equipment is simple, cost is low and feature to environment and mankind's nonhazardous, but extraction ratio is on the low side, and impurity content is high, and post-processing difficulty is large.Organic solvent especially ketone, alcohol extraction is followed the example of, and is quite classical method.Such as have by the method for acetone as extractant: (1) carbon tetrachloride extraction method (2) the Lead oxide hydrate sedimentation method.(1) method handicraft product flavone content is too low, does not reach standard; (2) although method can extract from Folium Ginkgo preferably active constituent content higher extract, there is a lot of shortcoming in them.Such as, employ butanone, the hazardous solvents etc. such as carbon tetrachloride, the residual of these materials cannot be avoided in product, complicated operation and step many, cause taking out greenery patches and the quality of end article is stable not, it is high that supercritical extraction has product yield, and quality is good, effective ingredient destroys less, no solvent residue, the advantage such as easy to operate.But supercritical fluid extraction equipment scale is comparatively large, technical requirement is high, investment is large, safety operation requirement is high, be difficult to use in large-scale production.
Summary of the invention
The present invention is directed to that traditional extraction yield is low, investment is large, impurity content is high and affect the problems such as product quality, propose flavone extracting method in a kind of Folium Ginkgo, the method extraction yield is high, cost of investment is few, without problems such as qualitative effects.
In order to reach above-mentioned purpose, the concrete technical scheme of employing is:
(1) cleaned by Folium Ginkgo, with the ultra violet lamp 1-2h of 50-60W, treat that Folium Ginkgo withers, percentage of water loss is that 70%-80% stops illumination, then puts it in constant temperature oven, under the protection of nitrogen at 40-45 DEG C dry 1-2h;
(2) jet mill is put in dried Folium Ginkgo taking-up to pulverize and sieve, sifting out its internal diameter is 100nm;
(3) by concentration be 70% alcoholic solution ammonium solid-liquid ratio 1:15 mix homogeneously, after temperature control water bath being set as 65 DEG C of lixiviate 1h, in the water-bath of 65 DEG C, ultrasonic assistant extracts 3 times, shakes 10min at every turn;
(4) kieselguhr adding 20g in the solution of above-mentioned extraction is filtered;
(5) filtrate of collecting is carried out distilling under reduced pressure with Rotary Evaporators at 65 DEG C until residual minority moisture, institute's extract matter is paste;
(6) dH is used 2o again dissolves and filters, and is settled to 100mL, carries out extraction 3 times with 100mL dichloromethane, then through resin purification, eluting, after the precipitation liquid recovery ethanol of gained, then obtains ginkgolide compound with alcohol crystal;
(7) by silicagel column in ginkgolide compound crystallization, with the mixed liquor eluting of normal hexane and ethyl acetate, Fractional Collections eluent, finally again carries out concentrating under reduced pressure by the solution after eluting at 60 DEG C, namely obtains red sticky flavone.
The significant advantage that the present invention has is:
1, utilize the irradiation of ultraviolet light, not destroying under the original material conditions of Folium Ginkgo, making it dry out, being conducive to the separation of inner organic substance;
2, the flavone extraction yield of this invention extraction is high, without the need to extracting with supercritical fluid under condition of high voltage.
Specific embodiments
(1) cleaned by Folium Ginkgo, with the ultra violet lamp 1-2h of 50-60W, treat that Folium Ginkgo withers, percentage of water loss is that 70%-80% stops illumination, then puts it in constant temperature oven, under the protection of nitrogen at 40-45 DEG C dry 1-2h;
(2) jet mill is put in dried Folium Ginkgo taking-up to pulverize and sieve, sifting out its internal diameter is 100nm;
(3) by concentration be 70% alcoholic solution ammonium solid-liquid ratio 1:15 mix homogeneously, after temperature control water bath being set as 65 DEG C of lixiviate 1h, in the water-bath of 65 DEG C, ultrasonic assistant extracts 3 times, shakes 10min at every turn;
(4) kieselguhr adding 20g in the solution of above-mentioned extraction is filtered;
(5) filtrate of collecting is carried out distilling under reduced pressure with Rotary Evaporators at 65 DEG C until residual minority moisture, institute's extract matter is paste;
(6) dH is used 2o again dissolves and filters, and is settled to 100mL, carries out extraction 3 times with 100mL dichloromethane, then through resin purification, eluting, after the precipitation liquid recovery ethanol of gained, then obtains ginkgolide compound with alcohol crystal;
(7) by silicagel column in ginkgolide compound crystallization, with the mixed liquor eluting of normal hexane and ethyl acetate, Fractional Collections eluent, finally again carries out concentrating under reduced pressure by the solution after eluting at 60 DEG C, namely obtains red sticky flavone.
Example 1
Cleaned by Folium Ginkgo, with the ultra violet lamp 1h of 50W, treat that Folium Ginkgo withers, percentage of water loss is 70% stopping illumination, then puts it in constant temperature oven, under the protection of nitrogen at 40 DEG C dry 1h; Jet mill is put in dried Folium Ginkgo taking-up pulverize and sieve, sifting out its internal diameter is 100nm; With the alcoholic solution ammonium solid-liquid ratio 1:15 mix homogeneously that concentration is 70%, after temperature control water bath being set as 65 DEG C of lixiviate 1h, in the water-bath of 65 DEG C, ultrasonic assistant extracts 3 times, shakes 10min at every turn; The kieselguhr adding 20g in the solution of above-mentioned extraction is filtered; The filtrate of collecting is carried out distilling under reduced pressure with Rotary Evaporators at 65 DEG C until residual minority moisture, institute's extract matter is paste; Use dH 2o again dissolves and filters, and is settled to 100mL, carries out extraction 3 times with 100mL dichloromethane, then through resin purification, eluting, after the precipitation liquid recovery ethanol of gained, then obtains ginkgolide compound with alcohol crystal; By silicagel column in ginkgolide compound crystallization, with the mixed liquor eluting of normal hexane and ethyl acetate, Fractional Collections eluent, carry out concentrating under reduced pressure at finally molten after eluting being pressed on 60 DEG C, namely obtain red sticky flavone.
Example 2
Cleaned by Folium Ginkgo, with the ultra violet lamp 1.5h of 55W, treat that Folium Ginkgo withers, percentage of water loss is 75% stopping illumination, then puts it in constant temperature oven, under the protection of nitrogen at 43 DEG C dry 1.5h; Jet mill is put in dried Folium Ginkgo taking-up pulverize and sieve, sifting out its internal diameter is 100nm; With the alcoholic solution ammonium solid-liquid ratio 1:15 mix homogeneously that concentration is 70%, after temperature control water bath being set as 65 DEG C of lixiviate 1h, in the water-bath of 65 DEG C, ultrasonic assistant extracts 3 times, shakes 10min at every turn; The kieselguhr adding 20g in the solution of above-mentioned extraction is filtered; The filtrate of collecting is carried out distilling under reduced pressure with Rotary Evaporators at 65 DEG C until residual minority moisture, institute's extract matter is paste; Use dH 2o again dissolves and filters, and is settled to 100mL, carries out extraction 3 times with 100mL dichloromethane, then through resin purification, eluting, after the precipitation liquid recovery ethanol of gained, then obtains ginkgolide compound with alcohol crystal; By silicagel column in ginkgolide compound crystallization, with the mixed liquor eluting of normal hexane and ethyl acetate, Fractional Collections eluent, carry out concentrating under reduced pressure at finally molten after eluting being pressed on 60 DEG C, namely obtain red sticky flavone.
Example 3
Cleaned by Folium Ginkgo, with the ultra violet lamp 2h of 60W, treat that Folium Ginkgo withers, percentage of water loss is 80% stopping illumination, then puts it in constant temperature oven, under the protection of nitrogen at 45 DEG C dry 2h; Jet mill is put in dried Folium Ginkgo taking-up pulverize and sieve, sifting out its internal diameter is 100nm; With the alcoholic solution ammonium solid-liquid ratio 1:15 mix homogeneously that concentration is 70%, after temperature control water bath being set as 65 DEG C of lixiviate 1h, in the water-bath of 65 DEG C, ultrasonic assistant extracts 3 times, shakes 10min at every turn; The kieselguhr adding 20g in the solution of above-mentioned extraction is filtered; The filtrate of collecting is carried out distilling under reduced pressure with Rotary Evaporators at 65 DEG C until residual minority moisture, institute's extract matter is paste; Use dH 2o again dissolves and filters, and is settled to 100mL, carries out extraction 3 times with 100mL dichloromethane, then through resin purification, eluting, after the precipitation liquid recovery ethanol of gained, then obtains ginkgolide compound with alcohol crystal; By silicagel column in ginkgolide compound crystallization, with the mixed liquor eluting of normal hexane and ethyl acetate, Fractional Collections eluent, carry out concentrating under reduced pressure at finally molten after eluting being pressed on 60 DEG C, namely obtain the concentrated of red sticky flavone.

Claims (1)

1. a flavone extracting method in Folium Ginkgo, is characterized in that:
(1) cleaned by Folium Ginkgo, with the ultra violet lamp 1-2h of 50-60W, treat that Folium Ginkgo withers, percentage of water loss is that 70%-80% stops illumination, then puts it in constant temperature oven, under the protection of nitrogen at 40-45 DEG C dry 1-2h;
(2) jet mill is put in dried Folium Ginkgo taking-up to pulverize and sieve, sifting out its internal diameter is 100nm;
(3) by concentration be 70% alcoholic solution ammonium solid-liquid ratio 1:15 mix homogeneously, after temperature control water bath being set as 65 DEG C of lixiviate 1h, in the water-bath of 65 DEG C, ultrasonic assistant extracts 3 times, shakes 10min at every turn;
(4) kieselguhr adding 20g in the solution of above-mentioned extraction is filtered;
(5) filtrate of collecting is carried out distilling under reduced pressure with Rotary Evaporators at 65 DEG C until residual minority moisture, institute's extract matter is paste;
(6) dH is used 2o again dissolves and filters, and is settled to 100mL, carries out extraction 3 times with 100mL dichloromethane, then through resin purification, eluting, after the precipitation liquid recovery ethanol of gained, then obtains ginkgolide compound with alcohol crystal;
(7) by silicagel column in ginkgolide compound crystallization, with the mixed liquor eluting of normal hexane and ethyl acetate, Fractional Collections eluent, finally again carries out concentrating under reduced pressure by the solution after eluting at 60 DEG C, namely obtains red sticky flavone.
CN201410631856.9A 2014-11-11 2014-11-11 Extraction method of flavonol in ginkgo leaves Pending CN104435017A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410631856.9A CN104435017A (en) 2014-11-11 2014-11-11 Extraction method of flavonol in ginkgo leaves

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410631856.9A CN104435017A (en) 2014-11-11 2014-11-11 Extraction method of flavonol in ginkgo leaves

Publications (1)

Publication Number Publication Date
CN104435017A true CN104435017A (en) 2015-03-25

Family

ID=52882279

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410631856.9A Pending CN104435017A (en) 2014-11-11 2014-11-11 Extraction method of flavonol in ginkgo leaves

Country Status (1)

Country Link
CN (1) CN104435017A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107413068A (en) * 2017-08-03 2017-12-01 广州韩能大健康产品有限公司 The method extracted using silicon element concentrate to effective ingredients in plant
CN107647407A (en) * 2017-11-14 2018-02-02 宜昌东方昌绿茶业有限公司 A kind of method that flavonol is extracted from ginkgo leave tea
CN108181254A (en) * 2018-02-11 2018-06-19 神威药业集团有限公司 A kind of ginkgo biloba p.e crude product column chromatography process for purification and application

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101134758A (en) * 2007-10-15 2008-03-05 桂林市振达生物科技有限责任公司 Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf
CN102911791A (en) * 2012-09-25 2013-02-06 常州亚环环保科技有限公司 Method for extracting gardenia essential oil

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101134758A (en) * 2007-10-15 2008-03-05 桂林市振达生物科技有限责任公司 Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf
CN102911791A (en) * 2012-09-25 2013-02-06 常州亚环环保科技有限公司 Method for extracting gardenia essential oil

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
徐华杰 等: "银杏叶总黄酮的提取和表征", 《阜阳师范学院学报(自然科学版)》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107413068A (en) * 2017-08-03 2017-12-01 广州韩能大健康产品有限公司 The method extracted using silicon element concentrate to effective ingredients in plant
CN107647407A (en) * 2017-11-14 2018-02-02 宜昌东方昌绿茶业有限公司 A kind of method that flavonol is extracted from ginkgo leave tea
CN108181254A (en) * 2018-02-11 2018-06-19 神威药业集团有限公司 A kind of ginkgo biloba p.e crude product column chromatography process for purification and application

Similar Documents

Publication Publication Date Title
CN1974527B (en) Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf
CN111807932A (en) Method for extracting and purifying cannabidiol from cannabis sativa
CN104710391B (en) Method for extracting luteolin and beta-sitosterol from peanut shells
CN101912480A (en) Method for preparing procyanidin extract of lycium ruthenicum murr
CN102432582A (en) Preparation method of proanthocyanidin
JP2017520616A (en) Extraction method of chlorogenic acid from Tochu leaves
CN105237537A (en) Method for preparing matrine and sophoridine in sophora alopecuroides
CN104435017A (en) Extraction method of flavonol in ginkgo leaves
CN103193832B (en) Method for extracting and separating high-purity tea polyphenol from tea leaves
CN107098942B (en) Method for subcritical water extraction of kaempferitrin in radish leaves
CN106854193A (en) A kind of preparation method that catechin is extracted from tealeaves
CN107684568A (en) Method for extracting and refining high-purity ginkgetin from ginkgo leaves
CN104095889B (en) A kind of preparation method of ginkgo biloba p.e
CN106727746A (en) The preparation method of low sour water soluble ginkgo leaf extract
CN104000935B (en) A kind of method that anti-oxidant phenolic acid is extracted in the slag from jacket
CN101352616B (en) Method for preparing pine tree bark extract using barrier separation integrated process engineering
CN104497057A (en) Process for extracting tea polyphenols from Yunan dayezhong tea leaves
CN101985440B (en) Method for producing piperine
CN103275049A (en) Method for preparing myricetin by using vine tea and application of pyrosulfite
CN109021042B (en) Method for extracting high-purity oleuropein from olive leaves
CN104230871B (en) A kind of method separating polymethoxyflavone in Fructus Aurantii Immaturus, Hesperidin and Neosynephrine
CN105294793A (en) Separation method for naringin in aizoon stonecrop herb
CN103271973A (en) Method for extracting total triterpenoid substances from cornel
CN101412724A (en) Method for extracting bilobalide compound from ginkgo leaf
CN102911185B (en) Method for separating and purifying ginkgolides A, B, C and D and bilobalide from ginkgo leaf extracts

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20150325

WD01 Invention patent application deemed withdrawn after publication