CN101422502A - Preparation method of dogwood extract containing ursolic acid - Google Patents
Preparation method of dogwood extract containing ursolic acid Download PDFInfo
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- CN101422502A CN101422502A CNA2008101628328A CN200810162832A CN101422502A CN 101422502 A CN101422502 A CN 101422502A CN A2008101628328 A CNA2008101628328 A CN A2008101628328A CN 200810162832 A CN200810162832 A CN 200810162832A CN 101422502 A CN101422502 A CN 101422502A
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- fructus corni
- ursolic acid
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- extract
- fermentation
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Abstract
The invention discloses a preparation method of an extract of dogwood containing ursolic acid, and the method comprises the following steps of: 1) mixing dogwood powder with water, then carrying out fermentation shaker to the mixture of the dogwood powder and water by inoculating grape wine microzyme, thus obtaining a zymotic fluid; 2) adding distilled water to the zymotic fluid, carrying out aqueous bath and then carrying out ultrasonication; 3) filtering the product obtained in the second procedure, and then carrying out ultrasonic extraction by adding ethanol to the obtained filter residue; carrying out pumping filtration and concentration to obtain a concentrated solution; and 4) extracting the concentrated solution by using sherwood oil, and then condensing and drying the substrate liquid, thus obtaining the extract of dogwood containing ursolic acid. The preparation method of the extract of dogwood containing ursolic acid has the advantages of low cost, simple technique, easiness for industrial production, environmental protection, etc.
Description
Technical field
The present invention relates to a kind of fermentation new method for processing of Fructus Corni, particularly utilize Fructus Corni to extract the method for ursolic acid, belong to the Food Chemistry field.
Background technology
Fructus Corni is Cornaceae plant Cornus officinalis Sieb.et Zucc, it is a kind of important wild resource, its meat flavour acid, puckery of fruit, tepor, return the Liver and kidney warp, the effect that liver and kidney tonifying, essence astringing and desertion stemming are arranged cures mainly vertigo and tinnitus, soreness of waist and knee joint, impotence and seminal emission, enuresis frequent micturition, profuse sweating collapse, interior-heat is quenched one's thirst, and is one of tcm clinical practice famous and precious traditional antiaging agent commonly used.Fructus Corni all has distribution and cultivation on China Zhejiang, Henan, Shanxi, Sichuan and other places, aboundresources, and extensive market, its market development economic benefit is considerable.
Ursolic acid is a kind of important chemical constituent in the cornus fruit, average content 0.234%.Ursolic acid has wide biological activity, comprises anticancer, the injury protection to liver, antiinflammatory, antibiotic, antioxidation etc., is one of main active in the cornus fruit, and its Study on extraction and the exploitation of new purposes are the focuses of this area research.
Polysaccharide also is important active substance in Fructus Corni, and content is higher.Is in the Fructus Corni extract of main active in preparation with the ursolic acid, and the removal of polysaccharide is an important step, methods such as many at present employing macroporous resin chromatographies; But this kind chromatography method is not easy to batch production production.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method that contains the Fructus Corni extract of ursolic acid, and this method has that cost is low, technology is simple, be easy to characteristics such as suitability for industrialized production, environmental friendliness.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method that contains the Fructus Corni extract of ursolic acid, may further comprise the steps:
1), powder of Fructus Corni is mixed with water, inoculate the wine yeast of powder of Fructus Corni weight 2%～4% then and carry out shaker fermentation, fermentation temperature is 25～35 ℃, fermentation time 4d～8d; Get fermentation liquid;
2), in fermentation liquid, add behind the distilled water in 50～70 ℃ of water-bath 0.5～2h, ultrasonic Treatment 1～3 time under the frequency of 50～70 ℃ and 30～40KHZ then, each ultrasonic treatment time is 10～20min;
3), filtration step 2) gains, adding volumetric concentration in the filtering residue of gained is 75%～95% ethanol, ultrasonic extraction 5～15min under the frequency of 40～60 ℃ and 30～40KHZ; Sucking filtration concentrates then, gets concentrated solution;
4), the concentrated solution petroleum ether extraction, get that subnatant concentrates and dry, obtain containing the Fructus Corni extract of ursolic acid.
Improvement as the preparation method of the Fructus Corni extract that contains ursolic acid of the present invention: every g powder of Fructus Corni is dissolved in 0.5～3ml water in the step 1).
Further improvement as the preparation method of the Fructus Corni extract that contains ursolic acid of the present invention: the rotating speed of shaker fermentation is 110rpm～150rpm in the step 1).
Further improvement as the preparation method of the Fructus Corni extract that contains ursolic acid of the present invention: the distilled water step 2) and the envelope-bulk to weight ratio of the powder of Fructus Corni in the step 1) are 20～60ml/g.
Further improvement as the preparation method of the Fructus Corni extract that contains ursolic acid of the present invention: the ethanol in the step 3) and the envelope-bulk to weight ratio of the powder of Fructus Corni in the step 1) are 20～60ml/g.
Further improvement as the preparation method of the Fructus Corni extract that contains ursolic acid of the present invention: the volume 1～2:3 of step 4) PetroChina Company Limited. ether and concentrated solution.
In the present invention, wine yeast can be selected Saccharomyces cerevisiaeATCC26497 for use, Saccharomyces cerevisiae ATCC9080, or wine yeast such as Saccharomycescerevisiae CICC1012.
The Fructus Corni extract that contains ursolic acid of the final gained of the present invention is a chip solid.
The invention belongs to a kind of fermentation new method for processing of Fructus Corni, its technical scheme mainly is: 1. utilized the wine yeast fermentation to remove sugar, thereby removed the soluble sugar in the raw material Fructus Corni; 2. utilize ursolic acid to be dissolved in that ethanol is water insoluble, the character of petroleum ether, adopt water and petroleum ether remove impurity, thereby improve the purity of ursolic acid in the product.
In the present invention, the capacity of round is selected 2～4 times of reaction system volume for use in the step 1).
Method of the present invention is compared with traditional method, and advantage is:
(1) the present invention adopts fermentation method to remove sugar, and method is easy, easy operating; And polysaccharide material can be converted into the available ethanol of this technology by fermentation; Because the recyclable utilization of ethanol, therefore method environmental friendliness of the present invention is pollution-free, can also reduce production costs.The Fructus Corni extract that contains ursolic acid of gained of the present invention is mainly used in the health food development field.
Though macroporous resin of the prior art removes sugared effect preferably except that sugared method also can reach, chromatographic technique is not easy-operating on the present large-scale industrial production, and requires extremely strict aspect food industry; Therefore be unsuitable for producing the Fructus Corni extract that contains ursolic acid.
(2) chromatography that the present invention is more traditional removes sugared technology and is easier to the industrialization operation.
(4) the present invention is an extractant with cheap, nontoxic ethanol, and ethanol can recycle, and has reduced production cost.
(5) this is in invention: behind gains filtration step 2), contain a small amount of ethanol in the filtrate of gained, recyclable utilization; Can further reduce production costs.
(6) the present invention uses petroleum ether in secondary remove impurity process, and its polarity is little, and boiling point is low, and impurity-eliminating effect is obvious, separates easily, is difficult for residual.
The specific embodiment
Embodiment 1, a kind of preparation method that contains the Fructus Corni extract of ursolic acid, carry out following steps successively:
1), get powder of Fructus Corni 45g and 25ml water uniform mixing, inoculate the wine yeast of 1.5g then and carry out shaker fermentation, fermentation temperature is 27 ℃, shaking speed 120rpm, fermentation time 6d; Get fermentation liquid.
2), in fermentation liquid, add 2500ml distilled water, 50 ℃ of water-bath 1h; (frequency: 30～40KHZ) handle 2 times, handle 15min at every turn at 50 ℃ of following ultrasound wave then.
3), filtration step 2) gains, discard filtrate (containing ethanol in this filtrate, recyclable utilization); Adding the 2500ml volumetric concentration in the filtering residue of gained is 95% ethanol, in 50 ℃ of ultrasound wave (frequency: 30～40KHZ) extraction 10min.Then, the solution filtration with gained discards filtering residue; With 75～85 ℃ of concentrating under reduced pressure of filtrate, until being 250ml; Get concentrated solution.
4), evenly divide above-mentioned concentrated solution in two the 250ml separatory funnels of packing into; Each separatory funnel is all carried out following operation: add the 63ml petroleum ether, shake up, leave standstill 10min, discard upper strata liquid, the gained subnatant is evaporated to pasty state for 60 ℃, 80 ℃ of drying under reduced pressure 4h of gained pasty state liquid, and getting 1.08g is the Fructus Corni extract of chip solid.
In this Fructus Corni extract, ursolic acid content is 10%.
Embodiment 2, a kind of preparation method that contains the Fructus Corni extract of ursolic acid, carry out following steps successively:
1), get powder of Fructus Corni 60g and add 100ml water uniform mixing, inoculate the wine yeast of 2.0g then and carry out shaker fermentation, fermentation temperature is 30 ℃, shaking speed 145rpm, fermentation time 4d; Get fermentation liquid.
2), in fermentation liquid, add 3000ml distilled water, 60 ℃ of water-bath 0.5h; (frequency: 30～40KHZ) handle 2 times, handle 15min at every turn at 60 ℃ of following ultrasound wave then.
3), filtration step 2) gains, discard filtrate; Adding the 3000ml volumetric concentration in the filtering residue of gained is 95% ethanol, in 60 ℃ of ultrasound wave (frequency: 30～40KHZ) extraction 10min.Then, the solution filtration with gained discards filtering residue; With 75 ℃ of concentrating under reduced pressure of filtrate, until being 300ml; Get concentrated solution.
4), evenly divide above-mentioned concentrated solution in two the 250ml separatory funnels of packing into; Each separatory funnel is all carried out following operation: add the 82ml petroleum ether, shake up, leave standstill 10min, discard upper strata liquid, the gained subnatant is evaporated to pasty state for 60 ℃, 80 ℃ of drying under reduced pressure 4h of gained pasty state liquid, and getting 1.3g is the Fructus Corni extract of chip solid.
In this Fructus Corni extract, ursolic acid content is 10.2%.
Embodiment 3, a kind of preparation method that contains the Fructus Corni extract of ursolic acid, carry out following steps successively:
1), get powder of Fructus Corni 75g and add 130ml water uniform mixing, inoculate the wine yeast of 2.5g then and carry out shaker fermentation, fermentation temperature is 35 ℃, shaking speed 130rpm, fermentation time 8d; Get fermentation liquid.
2), in fermentation liquid, add 3500ml distilled water, 60 ℃ of water-bath 2h; (frequency: 30～40KHZ) handle 2 times, handle 15min at every turn at 70 ℃ of following ultrasound wave then.
3), filtration step 2) gains, discard filtrate; Adding the 2500ml volumetric concentration in the filtering residue of gained is 85% ethanol, in 55 ℃ of ultrasound wave (frequency: 30～40KHZ) extraction 10min.Then, the solution filtration with gained discards filtering residue; With 75 ℃ of concentrating under reduced pressure of filtrate, until being 250ml; Get concentrated solution.
4), evenly divide above-mentioned concentrated solution in two the 250ml separatory funnels of packing into; Each separatory funnel is all carried out following operation: add the 80ml petroleum ether, shake up, leave standstill 10min, discard upper strata liquid, the gained subnatant is evaporated to pasty state for 60 ℃, 80 ℃ of drying under reduced pressure 4h of gained pasty state liquid, and getting 1.4g is the Fructus Corni extract of chip solid.
In this Fructus Corni extract, ursolic acid content is 10%.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (6)
1, a kind of preparation method that contains the Fructus Corni extract of ursolic acid is characterized in that may further comprise the steps:
1), powder of Fructus Corni is mixed with water, inoculate the wine yeast of powder of Fructus Corni weight 2%～4% then and carry out shaker fermentation, fermentation temperature is 25～35 ℃, fermentation time 4d～8d; Get fermentation liquid;
2), in fermentation liquid, add behind the distilled water in 50～70 ℃ of water-bath 0.5～2h, ultrasonic Treatment 1～3 time under the frequency of 50～70 ℃ and 30～40KHZ then, each ultrasonic treatment time is 10～20min;
3), filtration step 2) gains, adding volumetric concentration in the filtering residue of gained is 75%～95% ethanol, ultrasonic extraction 5～15min under the frequency of 40～60 ℃ and 30～40KHZ; Sucking filtration concentrates then, gets concentrated solution;
4), the concentrated solution petroleum ether extraction, get that subnatant concentrates and dry, obtain containing the Fructus Corni extract of ursolic acid.
2, the preparation method that contains the Fructus Corni extract of ursolic acid according to claim 1 is characterized in that: every g powder of Fructus Corni is dissolved in 0.5～3ml water in the described step 1).
3, the preparation method that contains the Fructus Corni extract of ursolic acid according to claim 2 is characterized in that: the rotating speed of shaker fermentation is 110rpm～150rpm in the described step 1).
4, the preparation method that contains the Fructus Corni extract of ursolic acid according to claim 3 is characterized in that: the distilled water described step 2) and the envelope-bulk to weight ratio of the powder of Fructus Corni in the step 1) are 20～60ml/g.
5, the preparation method that contains the Fructus Corni extract of ursolic acid according to claim 4 is characterized in that: the ethanol in the described step 3) and the envelope-bulk to weight ratio of the powder of Fructus Corni in the step 1) are 20～60ml/g.
6, the preparation method that contains the Fructus Corni extract of ursolic acid according to claim 5 is characterized in that: the volume 1～2:3 of described step 4) PetroChina Company Limited.'s ether and concentrated solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101628328A CN101422502A (en) | 2008-12-11 | 2008-12-11 | Preparation method of dogwood extract containing ursolic acid |
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| CNA2008101628328A CN101422502A (en) | 2008-12-11 | 2008-12-11 | Preparation method of dogwood extract containing ursolic acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747402B (en) * | 2009-12-28 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying malol in sedum kamtschaticum |
| US8748658B2 (en) | 2010-03-22 | 2014-06-10 | Council Of Scientific And Industrial Research | Fast isolation method for the natural scaffold ursolic acid from Diospyros melanoxylon |
| CN108467416A (en) * | 2018-06-21 | 2018-08-31 | 长沙爱扬医药科技有限公司 | The method that Fructus Corni extracts morroniside, loganin and ursolic acid |
| CN110283226A (en) * | 2019-08-06 | 2019-09-27 | 桂林莱茵生物科技股份有限公司 | A kind of method of antioxidant content in extraction rosemary |
| CN112442103A (en) * | 2020-11-11 | 2021-03-05 | 西安理工大学 | Natural PPAR gamma receptor agonist and preparation method and application thereof |
-
2008
- 2008-12-11 CN CNA2008101628328A patent/CN101422502A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747402B (en) * | 2009-12-28 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying malol in sedum kamtschaticum |
| US8748658B2 (en) | 2010-03-22 | 2014-06-10 | Council Of Scientific And Industrial Research | Fast isolation method for the natural scaffold ursolic acid from Diospyros melanoxylon |
| CN108467416A (en) * | 2018-06-21 | 2018-08-31 | 长沙爱扬医药科技有限公司 | The method that Fructus Corni extracts morroniside, loganin and ursolic acid |
| CN110283226A (en) * | 2019-08-06 | 2019-09-27 | 桂林莱茵生物科技股份有限公司 | A kind of method of antioxidant content in extraction rosemary |
| CN110283226B (en) * | 2019-08-06 | 2021-07-06 | 桂林莱茵生物科技股份有限公司 | Method for extracting antioxidant component in rosemary |
| CN112442103A (en) * | 2020-11-11 | 2021-03-05 | 西安理工大学 | Natural PPAR gamma receptor agonist and preparation method and application thereof |
| CN112442103B (en) * | 2020-11-11 | 2021-12-17 | 西安理工大学 | Natural PPAR gamma receptor agonist and preparation method and application thereof |
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Open date: 20090506 |