CN102040593A - Method for simultaneously extracting vitexin and quercetin from Chinese hawthorn leaf - Google Patents
Method for simultaneously extracting vitexin and quercetin from Chinese hawthorn leaf Download PDFInfo
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- CN102040593A CN102040593A CN2010102931635A CN201010293163A CN102040593A CN 102040593 A CN102040593 A CN 102040593A CN 2010102931635 A CN2010102931635 A CN 2010102931635A CN 201010293163 A CN201010293163 A CN 201010293163A CN 102040593 A CN102040593 A CN 102040593A
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Abstract
The invention relates to a method for simultaneously extracting vitexin and quercetin from Chinese hawthorn leaf, comprising the following steps: smashing raw materials; carrying out ultrasonic extraction for 2-3 times by alcoholic solution; decompressing extracting solution until no alcohol is contained; adding water for dispersing to the concentrated solution; then adding a macroporous resin column for adsorption; eluting with water and 40-70% alcohol solution; condensing the eluent, adding acid and hydrolyzing; filtering the condensed hydrolyzate; adding water to the precipitate for refluxing and dissolving; filtering while the obtained product is hot; respectively crystallizing and purifying solid and mother liquor; and drying in vacuum to obtain a vitexin product and a quercetin product. The process of the invention is simple operate, the obtained product has high purity, the utilization of the raw material is high, and the method is suitable for industrial production.
Description
Technical field:
The invention belongs to the Separation of Natural Products technical field, relate to a kind of method of from Howthorn Leaf, extracting Vitexin and Quercetin simultaneously.
Background technology:
Vitexin, flavonoid glycoside substance is dissolved in methyl alcohol, is soluble in hot water, is insoluble in benzene, chloroform, ether etc.
Quercetin has another name called quercetin, Quercetin, and the flavonols material, water insoluble, be soluble in organic solvent and oxyhydroxide alkaline solutions such as ethanol, methyl alcohol, ethyl acetate, chloroform, ether.
Howthorn Leaf is the dry leave of rosaceous plant Fruit of Pashi Pear or hawthorn.Has function promoting blood circulation and removing blood stasis, that regulate the flow of vital energy and promote blood circulation." Chinese pharmacopoeia 2005 editions has been recorded Howthorn Leaf and Folium Crataegi extract preparation---Yixintong sheet.Discover that flavones ingredient contained in the Howthorn Leaf has tangible pharmacological action to cardiovascular systems, mainly contains flavone components such as Vitexin glucoside, vitexin rhamnoside, rutin, Vitexin, Quercetin, Quercetin 3-galactoside.
Vitexin is mainly used in the treatment cardiovascular disorder, Vitexin purity general requirement＞98%.Existing patent medicine injection Vitexin is used for clinical treatment.The Vitexin major function is promoting blood circulation and removing blood stasis, regulates the flow of vital energy and promotes blood circulation.Be used for the obstruction of qi in the chest due to the hemostasis resistance arteries and veins, disease is seen chest distress, pareordia shouting pain, palpitation and amnesia, dizzy tinnitus.Disease persons such as coronary heart disease and angina pectoris, hyperlipidaemia, arteries and veins blood supply insufficiency aroused in interest.
Quercetin have preferably eliminate the phlegm, antitussive action, and certain antiasthmatic effect is arranged, be used for the treatment of chronic bronchitis.Bring high blood pressure down, strengthen capillary resistance in addition in addition, reduce effects such as capillary fragility, reducing blood-fat, coronary artery dilator, coronary blood flow increasing, antitumor action and platelet aggregation-against, coronary heart disease and hyperpietic are had the assisting therapy effect.Quercetin can be used as the main ancillary drug of treatment prostate cancer.Quercetin is one of the highest active compound in numerous flavonoid compounds.
Extracting Vitexin at present is to adopt Howthorn Leaf to refine, from Folium Crataegi total flavones, extract Vitexin through technologies such as extraction, separation, purifying, and finally make freeze-dried preparation, as disclosed method in the document " progress of Howthorn Leaf " is to adopt ethanol extract from water precipitation and solvent extration to extract, and extract separates with the silicagel column post through polyamide column and obtains Vitexin; As patent (application number: 200510038041.0) " extracting method of Vitexin, purposes and preparation ", the method of this patent disclosure is the crude extract hydrolysis in the aqueous solution under highly acid condition with Howthorn Leaf, after separating out crystallization, carry out recrystallization again, obtain the target product Vitexin.And the main source of Quercetin is rutin and Ginkgo Leaf, (application number: application number: 03133636.1) disclosed method is to utilize extensive and a large amount of rutins that exist in the natural plant in " the enzymatic hydrolysis rutin prepares the method for Quercetol 3-monoglucoside and Quercetin " as patent, adopt the part or all of glycosyl of enzymatic hydrolysis on it, and then preparation Quercetol 3-monoglucoside and Quercetin monomer; As patent (application number: 200810072848.X) " method that from cotton petal, prepares Quercetin ", the method of this patent disclosure is to be raw material with the cotton petal, through organic solvent extraction, acid or alkali are hydrolyzed, insulation, obtain the Quercetin crude product, obtain highly purified Quercetin by macroporous resin enrichment then.And from Howthorn Leaf, extract simultaneously extract Vitexin and Quercetin simultaneously method seldom.
Summary of the invention:
The present invention wants the technical solution problem to provide a kind of method of extracting Vitexin and Quercetin from Howthorn Leaf simultaneously.
The objective of the invention is to realize by following technical solution:
A kind of method of extracting Vitexin and Quercetin from Howthorn Leaf simultaneously is characterized in that comprising following steps:
1) preparation: raw material pulverizing, add 10-15 and doubly measure the alcoholic solution supersound extraction 2-3 time, extracting solution is evaporated to does not have alcohol, concentrated solution adds 3-5 times of water-dispersion, adds macroporous resin column absorption again, washes sugared reaction negative, doubly measure 40-70% ethanolic soln wash-out with 5-8 again, reclaim ethanol, get concentrated solution;
2) acid hydrolysis: above-mentioned concentrated solution adds acid and transfers the pH2-4 hydrolysis, and concentrating hydrolysate filters, and throw out is Vitexin and Quercetin;
3) separate: taking precipitate refluxes with 3-5 times of water gaging and dissolves, filtered while hot, and solids is the Quercetin crude extract, mother liquor is a Vitexin solution;
4) Quercetin purifying: above-mentioned Quercetin crude extract is refluxed dissolving crystallized 2-3 time with anhydrous methanol, and vacuum-drying promptly gets the Quercetin product;
5) Vitexin purifying: above-mentioned Vitexin solution is put cold crystallization, leach crystallization and reflux dissolving crystallized 2-3 time with dehydrated alcohol, the vacuum-drying crystallisate gets the Vitexin product.
Alcoholic solution in the described step 1) is methyl alcohol or the ethanolic soln of 60-90%, and supersound extraction power is 0.5-10kw, a kind of among the optional AB-8 of macroporous resin model, X-5, LSA-21 and the HZ806.
Described step 2) a kind of in sour optional hydrochloric acid, sulfuric acid and the phosphoric acid that uses in.
The present invention adopts the alcoholic solution supersound extraction, obtains the total flavones material through the macroporous resin column fractionation by adsorption, uses acid hydrolysis again, extract two kinds of active substances of Vitexin and Quercetin simultaneously, improved utilization ratio of raw materials, reduced cost, this technology has the industrialization meaning.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment:
Embodiment:
Embodiment 1:
Howthorn Leaf is pulverized, got 1kg, drop into extractor, added 15L90% ethanolic soln supersound extraction 1.5 hours, suction filtration liquid adds the 12L80% ethanolic soln again and extracts 1 time, obtain concentrated solution behind the extracting solution decompression recycling ethanol solution, concentrated solution adds the 4L water-dispersion, adds the absorption of 1L AB-8 macroporous resin column, flow velocity 2.5L/h, after absorption finishes, wash sugared reaction negative, use 7L60% ethanolic soln wash-out again, collect the elutriant decompression recycling ethanol and concentrate, concentrated solution adds sulfuric acid and transfers pH4, be heated to 7 ℃ of hydrolysis, hydrolyzed solution is concentrated into 1/5 volume, leaches throw out and adds 5L water backflow dissolving, filtered while hot, get solids 8.8g and mother liquor, solids refluxes with the 600ml dehydrated alcohol and dissolves, and places crystallization, crystallization refluxes with the 400ml anhydrous methanol and dissolves, place crystallization, leach crystallization vacuum-drying and promptly get Quercetin product 6.4g, content 93.7%; Above-mentioned mother liquor is put cold crystallization, leaches crystallization and refluxes dissolving crystallized 3 times with the 500ml anhydrous methanol, and the vacuum-drying crystallisate gets Vitexin product 7.2g, content 95.1%.
Embodiment 2:
Howthorn Leaf is pulverized, get 1kg, drop into extractor, added 12L60% ethanolic soln supersound extraction 2 hours, suction filtration liquid adds the 12L80% ethanolic soln again and extracts 2 times, obtains concentrated solution behind the extracting solution decompression recycling ethanol solution, concentrated solution adds the 3.5L water-dispersion, add the absorption of 1.5L LAS-21 macroporous resin column, flow velocity 1.5L/h is after absorption finishes, wash sugared reaction negative, use 6L70% ethanolic soln wash-out again, collect the elutriant decompression recycling ethanol and concentrate, concentrated solution adds sulfuric acid and transfers pH2, be heated to 80 ℃ of hydrolysis, hydrolyzed solution is concentrated into 1/6 volume, leaches throw out and adds 4L water backflow dissolving, filtered while hot, get solids 10.3g and mother liquor, solids refluxes with the 500ml anhydrous methanol and dissolves, and places crystallization, and crystallization refluxes dissolving crystallized 2 times with the 500ml anhydrous methanol again, leach crystallization vacuum-drying and promptly get Quercetin product 5.1g, content 92.0%; Organic solvent is removed in above-mentioned mother liquor decompression, refluxes dissolving crystallized 2 times with the 800ml dehydrated alcohol, and the vacuum-drying crystallisate gets Vitexin product 7.8g, content 94.2%.
Embodiment 3:
Howthorn Leaf is pulverized, got 1kg, drop into extractor, added 10L80% methanol solution supersound extraction 3 hours, suction filtration liquid adds the 12L70% methanol solution again and extracts 1 time, obtain concentrated solution behind the extracting solution decompression recycling ethanol solution, concentrated solution adds the 5L water-dispersion, adds the absorption of 2L X-5 macroporous resin column, flow velocity 3L/h, after absorption finishes, wash sugared reaction negative, use 5L60% ethanolic soln wash-out again, collect the elutriant decompression recycling ethanol and concentrate, concentrated solution adds hydrochloric acid and transfers pH2, be heated to 90 ℃ of hydrolysis, hydrolyzed solution is concentrated into 1/10 volume, leaches throw out and adds 5L water backflow dissolving, filtered while hot, get solids 8.2g and mother liquor, solids refluxes with the 700ml dehydrated alcohol and dissolves, and places crystallization, crystallization refluxes with the 500ml anhydrous methanol and dissolves, place crystallization, leach crystallization vacuum-drying and promptly get Quercetin product 5.9g, content 94.7%; Organic solvent is removed in above-mentioned mother liquor decompression, refluxes dissolving crystallized 3 times with the 500ml anhydrous methanol, and the vacuum-drying crystallisate gets Vitexin product 10.2g, content 98.0%.
Embodiment 4:
Howthorn Leaf is pulverized, got 1kg, drop into extractor, added 12L70% methanol solution supersound extraction 2 hours, suction filtration liquid adds the 10L70% ethanolic soln again and extracts 3 times, obtains concentrated solution behind the extracting solution decompression recycling ethanol solution, concentrated solution adds the 3.5L water-dispersion, add the absorption of 1.5LHZ806 macroporous resin column, flow velocity 1.5L/h is after absorption finishes, wash sugared reaction negative, use 8L40% ethanolic soln wash-out again, collect the elutriant decompression recycling ethanol and concentrate, concentrated solution adds phosphoric acid and transfers pH3, be heated to 85 ℃ of hydrolysis, hydrolyzed solution is concentrated into 1/6 volume, leaches throw out and adds 4L water backflow dissolving, filtered while hot, get solids 9.1g and mother liquor, solids refluxes with the 500ml dehydrated alcohol and dissolves, and places crystallization, and crystallization refluxes dissolving crystallized 2 times with the 500ml anhydrous methanol again, leach crystallization vacuum-drying and promptly get Quercetin product 7.1g, content 91.9%; Organic solvent is removed in above-mentioned mother liquor decompression, refluxes dissolving crystallized 2 times with the 500ml anhydrous methanol, and the vacuum-drying crystallisate gets Vitexin product 9.8g, content 91.3%.
Embodiment 5:
Howthorn Leaf is pulverized, get 1kg, drop into extractor, added 15L90% methanol solution supersound extraction 1 hour, suction filtration liquid adds the 12L80% methanol solution again and extracts 1 time, obtains concentrated solution behind the extracting solution decompression recycling ethanol solution, concentrated solution adds the 4L water-dispersion, add the absorption of 1L AB-8 macroporous resin column, flow velocity 2.5L/h is after absorption finishes, wash sugared reaction negative, use 6.5L50% ethanolic soln wash-out again, collect the elutriant decompression recycling ethanol and concentrate, concentrated solution adds sulfuric acid and transfers pH3, be heated to 70 ℃ of hydrolysis, hydrolyzed solution is concentrated into 1/10 volume, leaches throw out and adds 4.5L water backflow dissolving, filtered while hot, get solids 11.2g and mother liquor, solids refluxes with the 600ml dehydrated alcohol and dissolves, and places crystallization, and crystallization refluxes dissolving crystallized 2 times with the 400ml anhydrous methanol again, leach crystallization vacuum-drying and promptly get Quercetin product 9.2g, content 93.8%; Organic solvent is removed in above-mentioned mother liquor decompression, refluxes dissolving crystallized 3 times with the 550ml anhydrous methanol, and the vacuum-drying crystallisate gets Vitexin product 6.7g, content 96.1%.
Claims (3)
1. method of extracting Vitexin and Quercetin from Howthorn Leaf is characterized in that comprising following steps:
1) preparation: raw material pulverizing, add 10-15 and doubly measure the alcoholic solution supersound extraction 2-3 time, the no alcoholic solution of extracting solution decompression, concentrated solution adds 3-5 times of water-dispersion, adds macroporous resin column absorption again, washes sugared reaction negative, doubly measure 40-70% ethanolic soln wash-out with 5-8 again, reclaim ethanol, get concentrated solution;
2) acid hydrolysis: above-mentioned concentrated solution adds acid and transfers pH2-4, is heated to 70-90 ℃ of hydrolysis concentrating hydrolysate and filters, and throw out is Vitexin and Quercetin;
3) separate: taking precipitate refluxes with 3-5 times of water gaging and dissolves, filtered while hot, and solids is the Quercetin crude extract, mother liquor is a Vitexin solution;
4) Quercetin purifying: above-mentioned Quercetin crude extract is refluxed dissolving crystallized 2-3 time with anhydrous methanol, and vacuum-drying promptly gets the Quercetin product;
5) Vitexin purifying: above-mentioned Vitexin solution is put cold crystallization, leach crystallization and reflux dissolving crystallized 2-3 time with dehydrated alcohol, the vacuum-drying crystallisate gets the Vitexin product.
2. from Howthorn Leaf, put forward the method for Vitexin and Quercetin according to claim 1 simultaneously, it is characterized in that the alcoholic solution in the described step 1) is methyl alcohol or the ethanolic soln of 60-90%, supersound extraction power is 0.5-10kw, a kind of among the optional AB-8 of macroporous resin model, X-5, LSA-21 and the HZ806.
3. put forward the method for Vitexin and Quercetin according to claim 1 in the Howthorn Leaf simultaneously, it is characterized in that described step 2) in a kind of in the sour optional hydrochloric acid, sulfuric acid and the phosphoric acid that use.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659740A (en) * | 2012-04-26 | 2012-09-12 | 西安医学院 | Method for extracting quercetin from eucommia leaves |
| CN105237522A (en) * | 2015-10-16 | 2016-01-13 | 南京师范大学 | Method for preparing vitexin with Chinese prickly ash plants as raw materials |
| CN107029054A (en) * | 2017-06-21 | 2017-08-11 | 福建农林大学 | A kind of multiple-effect health care oral liquid and preparation method thereof |
| CN107281258A (en) * | 2017-07-19 | 2017-10-24 | 浙江大学 | A kind of beans taro leaf flavonoid extract and its preparation method and application |
| CN107721992A (en) * | 2017-09-08 | 2018-02-23 | 东北林业大学 | A kind of method for being converted from sorbic acid wastewater and separating Vitexin |
| CN108440477A (en) * | 2018-04-23 | 2018-08-24 | 江苏耐雀生物工程技术有限公司 | A method of preparing Quercetin from tungoiltree juvenile leaf |
| CN115894423A (en) * | 2022-12-30 | 2023-04-04 | 河北瑞龙生物科技有限公司 | Method for extracting quercetin from folium cortex eucommiae |
-
2010
- 2010-09-27 CN CN2010102931635A patent/CN102040593A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659740A (en) * | 2012-04-26 | 2012-09-12 | 西安医学院 | Method for extracting quercetin from eucommia leaves |
| CN102659740B (en) * | 2012-04-26 | 2014-04-02 | 西安医学院 | Method for extracting quercetin from eucommia leaves |
| CN105237522A (en) * | 2015-10-16 | 2016-01-13 | 南京师范大学 | Method for preparing vitexin with Chinese prickly ash plants as raw materials |
| CN107029054A (en) * | 2017-06-21 | 2017-08-11 | 福建农林大学 | A kind of multiple-effect health care oral liquid and preparation method thereof |
| CN107281258A (en) * | 2017-07-19 | 2017-10-24 | 浙江大学 | A kind of beans taro leaf flavonoid extract and its preparation method and application |
| CN107281258B (en) * | 2017-07-19 | 2020-12-11 | 浙江大学 | Doudouye flavonoid extract and preparation method and application thereof |
| CN107721992A (en) * | 2017-09-08 | 2018-02-23 | 东北林业大学 | A kind of method for being converted from sorbic acid wastewater and separating Vitexin |
| CN108440477A (en) * | 2018-04-23 | 2018-08-24 | 江苏耐雀生物工程技术有限公司 | A method of preparing Quercetin from tungoiltree juvenile leaf |
| CN115894423A (en) * | 2022-12-30 | 2023-04-04 | 河北瑞龙生物科技有限公司 | Method for extracting quercetin from folium cortex eucommiae |
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Application publication date: 20110504 |