CN101336978B - Extraction method of total flavone of Hovenia dulcisThunb - Google Patents
Extraction method of total flavone of Hovenia dulcisThunb Download PDFInfo
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Abstract
The invention discloses a method for extracting total flavonoids of hovenia dulcis. The method adopts the solvent extraction method and one optional method of the solvent extraction method, the macro-porous resin adsorption method, the supercritical fluid extraction method, the column chromatography or liquid-liquid countercurrent distribution chromatography, or the free combination of the methods. The total flavonoids of hovenia dulcis is extracted from any one part of hovenia acerba, such as fruit stems, fruits, seeds, seed-cases, leaves, flowers, roots, stems, branches, skins and fruit residues, etc., or the combination thereof and is further separated and purified. The prepared total flavonoids is a combination containing two or more flavonoid active components, wherein the total flavonoids comprises the main active components as follows: quercetin, kaempferol, myricetin, (+)-dihydromyricetin derivates, etc.; the total percentage composition of various flavonoid components by weight is 12% to 100%; and the preparation method is applicable to pharmaceutical industry, food industry, cosmetic industry and health-care product industry.
Description
Technical field
The present invention relates to a kind of extracting method, method of quality control of total flavone of Hovenia dulcisThunb and in the application of medicine, food, cosmetics and field of health care products, belong to the natural product field.
Background technology
Semen Hoveniae (Hovenia dulcis Thunb) is Rhamnaceae Semen Hoveniae (Fructus Hoveniae) platymiscium, and very abundant in china natural resources, its fruits and seeds with the meat fruit stem is used as medicine, and is called " Semen Hoveniae (Fructus Hoveniae) ", has alcoholic intoxication, the relieving restlessness of quenching the thirst, preventing or arresting vomiting, sharp defecation.Cure mainly drunk, excessive thirst, the vomiting, difficulty in urination and defecation, rheumatic numbness, the diseases such as contracture of the limbs.Semen Hoveniae leaf, flower, root, stem, branch, skin, juice have relieving alcoholic intoxication to calm the nerves, promote urine excretion, accelerate intestinal peristalsis promoting, dispelling wind and removing obstruction in the collateral relieving convulsion, the relieving restlessness of quenching the thirst, extra-nutrition, blood pressure lowering, tumor suppression, calmness, convulsion, protect the liver, the effect such as nourishing the liver, blood sugar lowering, among the people also with being used as medicine.
Flavone is the effective ingredient of Semen Hoveniae, and its primary structure is the chemical compound of the types such as flavonol (glycosides), flavonol and flavanone alcohols, have protect the liver, the effect such as alcoholic intoxication, antibiotic, antioxidation.
The solvent extraction process of at present existing bibliographical information Semen Hoveniae seed total flavonoid, but it just simply extracts total flavones, is not combined with additive method, carries out separation and the purification of total flavones crude extract, therefore general flavone content is all below 11% in the extract, and purity is very low; The preparation method that monomer flavone in the bibliographical information Semen Hoveniae fruit is also arranged, but it only extracts a kind of effective ingredient of flavone, does not relate to the total flavones preparation method; And the preparation method of other active sites of Semen Hoveniae such as leaf, flower, root, stem, branch, skin and pomace flavonoid all do not have bibliographical information, these all serious restriction the utilization of total flavone of Hovenia dulcisThunb and the performance of drug action.
Summary of the invention
The object of the present invention is to provide the extracting method of a kind of Semen Hoveniae, fruit stem, fruit, seed, kind shell, leaf, flower, root, stem, branch, skin and marc total flavones.
Another object of the present invention is to provide a kind of total flavone of Hovenia dulcisThunb as the application in medicine, food, cosmetics and field of health care products of pharmaceutical preparation, medicine adjuvant and functional factor.
Another object of the present invention is to provide that a kind of total flavone of Hovenia dulcisThunb can protect the liver as preparation or with some separately, relieves the effect of alcohol, antioxidation, antimicrobial drug share and make dosage form, is applied to medicine, foods and cosmetics and field of health care products.
The total flavone of Hovenia dulcisThunb that the present invention proposes, be the combination of two or more flavonoid active component of extracting from positions such as Semen Hoveniae, fruit stem, fruit, seed, kind shell, leaf, flower, root, stem, branch, skin or marcs, these compound structures are as follows:
Material of the present invention derives from Rhamnaceae Semen Hoveniae (Fructus Hoveniae) platymiscium Semen Hoveniae (Hovenia dulcisThunb).As the raw material that extracts total flavone of Hovenia dulcisThunb, it can be commercially available Semen Hoveniae, also can be arbitrary position or whole plant such as Semen Hoveniae fruit stem, fruit, seed, kind shell, leaf, flower, root, stem, branch, skin and marc, wherein preferred medical material position be Semen Hoveniae fruit stem, seed, leaf and marc.Semen Hoveniae described above comprises crude drug and the decoction pieces of processing without any process of preparing Chinese medicine, also comprises various processed products.
Total flavone of Hovenia dulcisThunb of the present invention refers to extract from any position of above-mentioned plant and obtains, and contains the compositions of following two or more flavonoid active component.These flavones ingredients comprise Quercetin, Quercetin-3-O-alpha-L-rhamnoside, 4 ', 5,7-trihydroxy-3 ', 5 '-dimethoxy flavone, ampelopsin, apiolin, Taxifolin, 3,4 ', 5,5 ', 7-penta hydroxy group-3 '-methoxy flavone, hovenodulinol, (+)-3,3 ', 5 ', 5,7-penta hydroxy group flavanone, kaempferol, kaempferol-3-O-alpha-L-rhamnoside, Kaempferol, 7-O-α-L-two rhamnosides, kaempferol-3-O-a-L-rhamnose-(1 → 6)-O-β-D-Glucose (1 → 2)-O-β-D-Glucose, kaempferol-3-o-α-L-rhamnose-7-O-[β-D-Glucose-(1 → 3)-α-L-rhamnose], dihydrokaempferol, (+)-dihydromyricetin, (+)-Jiao catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III, (-)-catechin, aromadendrin and afzelechin etc.
Among the various flavone components of Semen Hoveniae of the present invention, its topmost active component is Quercetin, kaempferol, ampelopsin, (+)-dihydromyricetin, hovenodulinol, (-)-catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III and aromadendrin etc. and derivant thereof etc.
As total flavone of Hovenia dulcisThunb, wherein the summation of each flavones ingredient percentage composition is 12～100% (W/W) by weight, wherein 50～100% (W/W) preferably.
Preparation total flavone of Hovenia dulcisThunb of the present invention except can be used for medical industry, also can be used for food industry, cosmetics industry and health product industry.
Preparation total flavone of Hovenia dulcisThunb of the present invention can make separately preparation or with other alcoholic intoxication, liver protecting and nourishing, antioxidation, the drug combination such as antibiotic, be used for the treatment of alcoholism, hepatopathy and because of the various diseases due to the free radical, these preparations have and whole identical or close pharmacologically active and the purposes of total flavone of Hovenia dulcisThunb.
The invention allows for the total flavone of Hovenia dulcisThunb extracting method, arbitrary position or its combinations such as Semen Hoveniae fruit stem, fruit, seed, kind shell, leaf, flower, root, stem, branch, skin and fruit stem marc, its adopts solvent extraction method and following any one method, or the combination in any of these methods is carried out the total flavone of Hovenia dulcisThunb extraction: 1. solvent extraction; 2. Flavonoids by Macroporous Adsorption Resin; 3. supercritical fluid extraction; 4. column chromatography; 5. liquid-liquid adverse current partography; Flavonoids by Macroporous Adsorption Resin preferably wherein.
When these methods of use are carried out the total flavone of Hovenia dulcisThunb extraction, generally comprise following one or several step:
(1) extract: solvent for use can be water or any one alcohols, ketone or esters solvent, or the mixed solvent that forms by a certain percentage of these solvents, or the acidity or the basic solvent that are made into by these solvents and acid, alkali, salt.Extracting method can be decoction, reflux, Soxhlet extraction, supersound extraction, merceration, seepage, microwave extraction, high pressure extract etc.
Preferred soxhlet extraction technique is: with 0～95% alcoholic solution (V/V), and take solid-liquid ratio as 1: 10～50 (g/mL), 60～100 ℃ of laser heating reflux, extract, 5～12h.
Preferred ultrasonic extraction technique is: Semen Hoveniae is extracted material pack in the supersound extraction device, be that 1: 6～15 (g/mL) add 0～95% alcoholic solution (V/V) by solid-liquid ratio, adopting temperature is 30～50 ℃, and frequency is that 40kHz, power are 0.3～0.5W/cm
2Ultrasonic extraction 15～30 minutes, extract merge extractive liquid, 2～3 times.
Preferred microwave extraction method technique is: add 0～95% alcoholic solution (V/V) with solid-to-liquid ratio 1: 20～40 (g/mL) and soaked 20～60 minutes, the control microwave power is 900W, shone 30～50 seconds, be cooled to rapidly room temperature after the taking-up, shone again 20～40 seconds, repeat 3～5 times with the method operation, filter merge extractive liquid.
(2) filter: comprise the methods such as centrifugal, sucking filtration, ultrafiltration, filter pressing, use or do not use following any one clarifier or its combination: the precipitate with ethanol agent, gelatin, Kaolin, various resins, Polyethylene Glycol, poly-second triol, chitosan and natural clarifying agent finished product are such as 101 fruit juice clarifiers, ZTC+1 natural clarifying agent etc.
Preferred clarifier is kieselguhr, be 1: 2～5 in extracting solution, to add kieselguhr according to kieselguhr and extract weight ratio, 10～50 ℃ of stir process 20～60min, then filter and obtain filtrate, recycling methanol, ethanol, chloroform, ether or wherein two or more acquisition of combination flushing clarifiers eluents, filtrate and eluent merging.
(3) concentrated: as to comprise thin film evaporation, rotary evaporation and decocting and concentrating etc. under normal pressure or the reduced pressure.
(4) drying: comprise vacuum drying, spray drying, lyophilization etc.
When adopting extraction to be prepared to carry out, generally first extract mixture is suspended from the water, then use alkanes (such as petroleum ether, hexane, gasoline etc.) extraction to remove oil-soluble impurities, then use suitable solvent, such as ether, chloroform, ethyl acetate, acetone, n-butyl alcohol etc., or the mixture of these solvents, extraction obtains total flavones composition wherein, obtains extractive of general flavone.
When adopting Flavonoids by Macroporous Adsorption Resin to be prepared, used macroporous resin can be any one types such as nonpolar, low pole, middle polarity, alkalescence or faintly acid, such as D101, D4020, D3500, D941, D21, HP-20, HP-20, XDA-1, AB-8, HPD400, S-8, HZ-806, H-50, H-30, LX-38, LX-28, LS-300B, LS-306, LSD-958, PA etc., the resin of low pole or middle polarity preferably wherein is such as LX-38, D101, AB-8 etc.Used eluant is water and moisture ethanol, methanol, acetone etc., wherein 50～95% alcoholic solution (V/V) preferably.
Preferred total flavone of Hovenia dulcisThunb extract resin purification technique is: select LX-38, D101, the AB-8 resin is as the purification resin, the thick total flavones of Semen Hoveniae is in crude drug amount (g)): the sample solution extension rate of dispersion milliliter number 1: 4～1: 18, absorption flow velocity 2～9BV/h, resin column blade diameter length ratio 1: 3～1: 10, applied sample amount is 100～500mg/mL (in the crude drug amount), 2～5 times of resin volumes of 0～20% alcoholic solution (V/V) eluting carry out remove impurity, the remove impurity flow velocity is 2～7BV/h, with 3～10 times of resin volumes of 50～95% alcoholic solution (V/V) eluting, elution flow rate is 2～9BV/h.
When adopting supercritical fluid extraction to be prepared, can directly extract the Semen Hoveniae raw material, also can the product that above-mentioned either method and step obtain be extracted.Can use or not use following any kind solvent and solvent mixture during extraction: water, alcohols, ketone, esters and ether solvents.
When adopting column chromatography to be prepared, the object of its processing can be the product that the said extracted step obtains, and also can be the product behind above-mentioned solvent extraction method, solvent extraction, Flavonoids by Macroporous Adsorption Resin or supercritical fluid extraction preliminary purification.Used immobile phase can be silica gel, polyamide, aluminium oxide, glucosan (Sephadex series or Sephadex-20 series), C-8, C-18, activated carbon, cellulose etc., used eluent generally is the mixed solvent that water, methanol, ethanol, acetone, chloroform, ethyl acetate, petroleum ether etc. form because the difference of immobile phase is different.Polyamide column chromatography preferably wherein.
The polyamide column chromatography purifying process is: select polyamide, Semen Hoveniae crude extract sample solution concentration 1: 4～1: 16 (with crude drug amount (g): disperse a milliliter number), absorption flow velocity 3～8BV/h, resin column blade diameter length ratio 1: 6～1: 20, applied sample amount is 100～500mg/mL (in the crude drug amount), 1～5 times of resin volume of 0～10% alcoholic solution (V/V) eluting carries out remove impurity, the remove impurity flow velocity is 3～7BV/h, with 4～7 times of resin volumes of 50～95% alcoholic solution (V/V) eluting, elution flow rate is 2～9BV/h, collects eluent, decompression and solvent recovery, the residue drying under reduced pressure gets total flavone of Hovenia dulcisThunb.
When adopting liquid-when the liquid counter-current extraction is prepared, the object of its processing can be the product of said extracted step, also can be the product behind above-mentioned solvent extraction method, solvent extraction, Flavonoids by Macroporous Adsorption Resin, supercritical fluid extraction and column chromatography preliminary purification.Generally be that extract mixture is suspended from the water, then remove oil-soluble impurities with alkanes or ether solvent (such as petroleum ether, hexane, the gasoline etc.) extraction of low polarity, then use the solvent of suitable polarity, such as chloroform, ethyl acetate, acetone, n-butyl alcohol etc., or the mixture of these solvents, extraction obtains total flavones composition wherein, gets total flavone of Hovenia dulcisThunb.
This total flavone of Hovenia dulcisThunb can be separately or with other any Chinese medicine and western medicine, food or adjuvant compatibility in any proportion, for the preparation of medicine, food, cosmetics and health product, the medicine of gained, food, cosmetics and health product can be capsule, tablet, pill, granule, oral liquid, syrup, electuary, medicated wine, injection, unguentum, powder, beverage etc.
Method of quality control of the present invention can comprise one or more in the following content assaying method:
1. total flavones
Precision takes by weighing 120 ℃ of control substance of Rutin 250mg that are dried to constant weight, with the absolute methanol dissolving, is transferred in the 250mL volumetric flask, uses the absolute methanol standardize solution, shakes up.Accurately pipette 5.00mL and place the 50mL volumetric flask, use the absolute methanol standardize solution, shake up.This control substance of Rutin solution concentration is 0.1mg/mL.Accurately draw 0.1mg/mL control substance of Rutin solution 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL, place respectively the 25mL volumetric flask, respectively add 50% alcoholic solution (V/V) to 6mL, add respectively 5% sodium nitrite solution (W/V) 1.00mL, shake up, add respectively 10% aluminum nitrate solution (W/V) 1.00mL after placing 6min, shake up, place 6min, add respectively again 1% sodium hydroxide solution 10.00mL, use again 50% alcoholic solution (V/V) standardize solution, shake up, behind the placement 15min, take blank solution as reference, survey absorbance at wavelength 510nm place, get regression equation.
Accurately draw respectively each 3 parts in Semen Hoveniae (Fructus Hoveniae) flavone extract sample, every part of 20mg puts in the 50mL volumetric flask, adds 50% alcoholic solution (V/V) ultrasonic dissolution and is diluted to scale, shakes up.Measure its absorbance A by the above colour developing and at 510nm wavelength place, by general flavone content in the regression equation calculation sample.
2. the content of hovenodulinol, Quercetin, aromadendrin and kaempferol
Chromatographic condition: chromatographic column: anti-phase C18 (4.6 * 250mm, 5 μ m); Mobile phase: 30～85% methanol solutions (V/V) (transferring pH to 3.0 with phosphoric acid) eluting (0～20min); Flow velocity: 1.0mL/Min; Detect wavelength: 360nm; Column temperature: room temperature.
Specification Curve of Increasing: the accurate absorption takes by weighing hovenodulinol, Quercetin, aromadendrin and kaempferol reference substance respectively, being mixed with respectively concentration with dissolve with methanol is 100,288,190 μ g/mL reference substance solution, 0,2,5,10,15,20 μ L injection liquid chromatographies, measure each chromatograph peak-to-peak area, take contrast sample size (μ g) as abscissa, chromatographic peak area is vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of extractive of general flavone samples, every part of about 20mg, place the 50mL measuring bottle, add the methanol ultrasonic dissolution, and be diluted to scale, shake up, test sample solution as hovenodulinol, Quercetin, aromadendrin and kaempferol assay, the above-mentioned test sample solution 20 μ L injection liquid chromatographies of accurate absorption are measured each chromatograph peak-to-peak area, calculate content.
3. dihydromyricetin
Chromatographic condition: chromatographic column: anti-phase C18 (4.6 * 250mm, 5 μ m); Mobile phase: 25～40% methanol solutions (V/V) (transferring pH to 3.0 with phosphoric acid) eluting (0～50min); Flow velocity: 1.0mL/Min; Detect wavelength: 294nm; Column temperature: room temperature.
Specification Curve of Increasing: precision is drawn (+)-dihydromyricetin reference substance solution (2.0 μ g/ μ L) 0,2,5,10,15,20 μ L injection liquid chromatographies respectively, measure each chromatograph peak-to-peak area, take contrast sample size (μ g) as abscissa, chromatographic peak area is vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of extractive of general flavone samples, every part of about 20mg, place the 50mL measuring bottle, add 20% acetonitrile solution (V/V) ultrasonic dissolution, and be diluted to scale, shake up, test sample solution as (+)-dihydromyricetin assay, the above-mentioned test sample solution 20 μ L injection liquid chromatographies of accurate absorption are measured each chromatograph peak-to-peak area, calculate content.
4. ampelopsin
Chromatographic condition: chromatographic column: anti-phase C18 (4.6 * 250mm, 5 μ m); Mobile phase: 40～60% methanol solutions (V/V) (transferring pH to 3.0 with phosphoric acid) eluting (0～50min); Flow velocity: 1.0mL/Min; Detect wavelength: 370nm; Column temperature: room temperature.
Specification Curve of Increasing: precision takes by weighing ampelopsin reference substance 9.80mg, puts in the 100mL volumetric flask, with dissolve with methanol and be settled to scale, shakes up, in contrast product solution.With methanol dilution and be settled to scale, shake up, be made into the ampelopsin solution injection liquid chromatography of 9.8,19.6,29.4,39.2,49.0 μ g/mL series concentration, measure each chromatograph peak-to-peak area, take contrast sample size (μ g) as abscissa, chromatographic peak area is vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of extractive of general flavone samples, every part of about 20mg, place the 50mL measuring bottle, add the methanol ultrasonic dissolution, and be diluted to scale, shake up, test sample solution as the ampelopsin assay, the above-mentioned test sample solution 20 μ L injection liquid chromatographies of accurate absorption are measured each chromatograph peak-to-peak area, calculate content.
4. catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III
Chromatographic condition: chromatographic column: anti-phase C18 (4.6 * 250mm, 5 μ m); Mobile phase: 15～60% (0～40min) methanol solution (V/V) eluting; Flow velocity: 1.0mL/Min; Detect wavelength: 280nm.Specification Curve of Increasing: precision is drawn catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III reference substance solution (0.027 μ g/ μ L) 0,2,5,10,15,20 μ L injection liquid chromatographies respectively, measure each chromatograph peak-to-peak area, take contrast sample size (μ g) as abscissa, chromatographic peak area is vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of extractive of general flavone samples, every part of about 20mg, place the 50mL measuring bottle, with 50% methanol aqueous solution (V/V) ultrasonic dissolution, and be diluted to scale, shake up, test sample solution as catechin and Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III assay, the above-mentioned test sample solution 20 μ L injection liquid chromatographies of accurate absorption are measured each chromatograph peak-to-peak area, calculate content.
The specific embodiment
Embodiment 1: the extraction of total flavone of Hovenia dulcisThunb
Get Semen Hoveniae leaf 1Kg and be crushed to 50 orders, solid-liquid ratio according to 1: 50 (g/mL) adds 75% alcoholic solution (V/V), laser heating reflux, extract, 9h, reclaim solvent and remove ethanol, regulate the pH=6 of extracting solution, the macroporous resin LSD-958 that has handled well on the filtrate, aqueous solution and 3 times of resin bed volume 20% alcoholic solution (V/V) flushing remove impurity with 4 times of resin bed volumes, flushing liquor discards, 95% alcoholic solution (V/V) eluting with 7 times of resin bed volumes, collect eluent, be concentrated into the dry total flavone of Hovenia dulcisThunb that gets of thick paste.Measuring total flavone of Hovenia dulcisThunb content is 66%, wherein Quercetin, kaempferol, ampelopsin, (+)-dihydromyricetin, hovenodulinol, (-)-catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III and aromadendrin etc. and derivant equal size thereof and be 51%.
Embodiment 2: the extraction of total flavone of Hovenia dulcisThunb
Get the sub-1Kg of ripe dry Semen Hoveniae and be crushed to 60 orders, 1: 40 (g/mL) added distilled water immersion 40 minutes with solid-to-liquid ratio, and the control microwave power is 900W, shone 50 seconds, and be cooled to rapidly room temperature after the taking-up, shone again 20 seconds, repeat 3 times with the method operation, filter merge extractive liquid.Extracting solution is evaporated to 20% (V/V), and it is suspended in water, then uses successively normal hexane, ethyl acetate extraction, reclaims respectively solvent and keeps extractive with organic solvent.Get acetic acid ethyl ester extract and use dissolve with ethanol, add kieselguhr according to 30% of weight, stirring at room was processed 30 minutes, and filtration is also used washing with alcohol, merging filtrate, the dry total flavone of Hovenia dulcisThunb that gets of vacuum concentration.The content of measuring total flavones is 87%, wherein Quercetin, kaempferol, ampelopsin, (+)-dihydromyricetin, hovenodulinol, (-)-catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III and aromadendrin etc. and derivative content thereof and be 63%.
Embodiment 3: the extraction of total flavone of Hovenia dulcisThunb
Get the dry marc 1Kg after the Semen Hoveniae (Fructus Hoveniae) fruit stem removes juice, pulverize, cross 100 mesh sieves, the impurity such as filtering cellulose, powder for drying, 80 ℃ of hot refluxs of 70% alcoholic solution (V/V) of 8 times of amounts (g/mL) are extracted each 2 hours 3 times, merging filtrate, vacuum concentration is removed ethanol, and extract adds 3 times of dissolved in distilled water by weight, upper polyamide chromatographic column, absorption flow velocity 5BV/h, polyamide column blade diameter length ratio 1: 8, applied sample amount are 400mg/mL (in the crude drug amount), and it is closely colourless to wash first outflow with water, use again 4 times of resin bed volume 30% alcoholic solution (V/V) flushing remove impurity, flushing liquor discards, and with 95% alcoholic solution (V/V) eluting of 5 times of polyamide bed volumes, elution flow rate is 4BV/h, collect eluent, be evaporated to the dry total flavone of Hovenia dulcisThunb that gets of thick paste.The content of measuring total flavones is 75%, wherein Quercetin, kaempferol, ampelopsin, (+)-dihydromyricetin, hovenodulinol, (-)-catechin, Semen Hoveniae (Fructus Hoveniae) element I, trifoliate orange root element II, Semen Hoveniae (Fructus Hoveniae) element III and aromadendrin etc. and derivative content thereof and be 52%.
Embodiment 4: the extraction of total flavone of Hovenia dulcisThunb
Getting ripe dry Semen Hoveniae (Fructus Hoveniae) seed 1Kg pulverizes, cross 100 mesh sieves, add 7 times of amounts (g/mL), 70% alcoholic solution (V/V), reflux, extract, 3 times, each 2 hours, the concentrated ethanol of removing of extracting solution, it is suspended in water, petroleum ether extraction is removed the impurity such as pigment, LX-38 type macroporous resin column on the aqueous extract, slowly loading, wash first 4 posts with water and stay volume, use 5 times of posts of 10% alcoholic solution (V/V) eluting instead and stay volume, use at last 95% alcoholic solution (V/V) eluting, work as 10%AlCl
3Solution (W/V) stops to collect when being detected as feminine gender, merges 95% alcoholic solution (V/V) eluting solvent, the dry total flavone of Hovenia dulcisThunb that gets of vacuum concentration.The content of measuring total flavones is 81%, wherein Quercetin, kaempferol, ampelopsin, (+)-dihydromyricetin, hovenodulinol, (-)-catechin, Semen Hoveniae (Fructus Hoveniae) element I, Semen Hoveniae (Fructus Hoveniae) element II, Semen Hoveniae (Fructus Hoveniae) element III and aromadendrin etc. and derivative content thereof and be 67%.
Embodiment 5: the preparation of total flavone of Hovenia dulcisThunb sheet
Total flavone of Hovenia dulcisThunb 10g
Starch 10g
The said components mix homogeneously, it is an amount of to add Pulvis Talci, is pressed into 100.
Embodiment 6: the preparation of total flavone of Hovenia dulcisThunb compound preparation
Total flavone of Hovenia dulcisThunb 20g
Flos puerariae lobatae flavone 15g
The said components mix homogeneously, in the hard gelatin capsule of packing into, totally 100 capsules.
Embodiment 7: the preparation of total flavone of Hovenia dulcisThunb compound preparation
Total flavone of Hovenia dulcisThunb 10g
Herba chloranthi japonici extract 10g
Herba Duchesneae Indicae extract 10g
The said components mix homogeneously is made 100 granules.
Claims (1)
1. the extracting method of a total flavone of Hovenia dulcisThunb, it is characterized in that, may further comprise the steps: get Semen Hoveniae leaf 1kg and be crushed to 50 orders, according to 1: the solid-liquid ratio of 50g/mL adds 75% alcoholic solution (V/V), laser heating reflux, extract, 9h, reclaim solvent and remove ethanol, regulate the pH=6 of extracting solution, the macroporous resin LSD-958 that has handled well on the filtrate, with aqueous solution and 3 times of resin bed volume 20% alcoholic solution (V/V) flushing remove impurity of 4 times of resin bed volumes, flushing liquor discards, with 95% alcoholic solution (V/V) eluting of 7 times of resin bed volumes, collect eluent, be concentrated into the dry total flavone of Hovenia dulcisThunb that gets of thick paste.
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| KR101713526B1 (en) * | 2015-08-17 | 2017-03-09 | 농업회사법인 주식회사 생명의나무 | Compositions for treatment, prevention or improvement of hepatotoxicity comprising taxifolin from seed of Hovenia dulcis |
| WO2017188759A2 (en) * | 2016-04-27 | 2017-11-02 | 경상대학교산학협력단 | Method for preparing hovenia dulcis extract with increased content of specific flavonoid and polyphenol compound |
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| CN107184452A (en) * | 2017-05-13 | 2017-09-22 | 吴杰 | A kind of preparation method, method of testing and the application of tealeaves general flavone |
| CN107903233A (en) * | 2018-01-08 | 2018-04-13 | 遵义医学院 | A kind of method of extraction separation myricetin and dihydromyricetin from HERBA SHUTERIAE |
| CN108330000B (en) * | 2018-04-09 | 2022-03-01 | 上海烟草集团有限责任公司 | A radix Seu folium Bergeniae extract and its preparation method and application |
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|---|---|---|---|---|
| CN101336987A (en) * | 2008-08-12 | 2009-01-07 | 西北农林科技大学 | Preparation method of total flavone of Hovenia dulcisThunb |
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Non-Patent Citations (3)
| Title |
|---|
| 丁林生等.枳椇子黄酮类成分研究.《药学学报》.1997,第32卷(第8期), * |
| 文为等.枳椇子总黄酮提取工艺的优化.《医药导报》.2008,第27卷(第1期),77-79. * |
| 梁侨丽等.枳椇叶的化学成分研究.《中草药》.1996,第27卷(第10期), * |
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