CN101817863A - Method for extracting ursolic acid from sea-buckthorn - Google Patents
Method for extracting ursolic acid from sea-buckthorn Download PDFInfo
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- CN101817863A CN101817863A CN200910216298A CN200910216298A CN101817863A CN 101817863 A CN101817863 A CN 101817863A CN 200910216298 A CN200910216298 A CN 200910216298A CN 200910216298 A CN200910216298 A CN 200910216298A CN 101817863 A CN101817863 A CN 101817863A
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- ursolic acid
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- buckthorn
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a technique for extracting ursolic acid, in particular to a method for extracting ursolic acid from sea-buckthorn, which comprises the following steps of: (1) preprocessing sea-buckthorn fruit; (2) extracting ursolic acid and oleanolic acid; and (3) separating the ursolic acid from the oleanolic acid. Compared with the prior art, the method for ursolic acid from the sea-buckthorn has the advantages that: a supercritical CO2 extraction method is used to extract the ursolic acid and the oleanolic acid from the peel of the sea-buckthorn fruit; the optimum distribution of resources is realized; and the added value of hippophae products is improved. In the invention, as the ursolic acid and the oleanolic acid are geometric isomers of triterpenic acids and have similar structures with the triterpenic acids, the ursolic acid and the oleanolic acid are separated by reversed phase high-performance liquid chromatography.
Description
Technical field
The present invention relates to the ursolic acid extractive technique, specifically relate to a kind of method of from sea-buckthorn, extracting ursolic acid.
Background technology
Ursolic acid is a kind of triterpene compound that is present in the natural phant, have various biological effects such as calmness, anti-inflammatory, antibiotic, anti-diabetic, antiulcer agent, lowering blood glucose, ursolic acid also has tangible anti-oxidant function, thereby is widely used as medicine and cosmetic material.
Studies show that ursolic acid also has and protect the liver in recent years, anti-hepatitis, antitumor action, antibiotic, anti-inflammatory and antiviral, reducing blood-fat, atherosclerosis, lowering blood glucose, inhibition, anti-diabetic, antiulcer agent, calmness, stable and raise immunity effect to hiv virus, evidence, ursolic acid is the enhancing body immunologic function obviously.The antitumor action that ursolic acid is described is extensive, very likely becomes the effective new type anticancer medicine of low toxicity.
The traditional extraction process of ursolic acid is Loquat Leaf or the Leaf of Glossy Privet alcohol reflux that will pulverize, obtain the flowing soaking paste extract, reclaim ethanol, said extracted thing water thorough washing after drying obtains dry extract, dry extract dissolve with ethanol rear decoloring, destainer adds elutriation and goes out a large amount of precipitations after reclaiming ethanol, adjust pH is to 2-2.5, separates, the collecting precipitation thing, and is washed with water to neutrality, vacuum-drying obtains the crude extract that major ingredient is a ursolic acid.
Because ursolic acid and Oleanolic Acid are triterpenic acid class isomers, structural similitude for better ursolic acid and the Oleanolic Acid of separating, adopt the chromatographic column of external leading company to separate.
Summary of the invention
The purpose of this invention is to provide a kind of ursolic acid extractive technique, specifically from seabuckthorn fruit peel, utilize supercritical CO
2Extraction process extracts the method for ursolic acid.
A kind of method of extracting ursolic acid from sea-buckthorn of the present invention is achieved by following technical proposals: a kind of method of extracting ursolic acid from sea-buckthorn of the present invention, it is characterized in that: described method comprises the steps:
(1) after the pre-treatment of sea buckthorn fruit is the cleaning of sea buckthorn fruit process, centrifuging and taking juice, obtains the process of fruit juice, seed of Fructus Hippophae and seabuckthorn fruit peel;
(2) extraction of ursolic acid and Oleanolic Acid is that seabuckthorn fruit peel is through degreasing, supercritical CO
2Extraction, get supernatant liquor after centrifugal, measure the ursolic acid content of target product in the supernatant liquor, promptly get crude extract after the drying; Extraction conditions is: 25 ℃ of extraction temperature, extracting pressure 25MPa, carry agent (this carries agent is dehydrated alcohol) 100ml, ethanol volume fraction 90%, target extract leaching yield is 288mg/100g.
(3) be to utilize reversed-phased high performace liquid chromatographic separating of ursolic acid and Oleanolic Acid, with the two separation.Concrete grammar is as follows: chromatographic column: Nucleosil C
18Post; Moving phase: 85: 15 methanol-water; Detect wavelength: 210nm; Flow velocity: 0.8ml/min; Column temperature: 25 ℃; Sample size: 20 μ l; External standard method quantitative analysis, ursolic acid and Oleanolic Acid theoretical tray number average greater than 10000, two component resolution greater than 1.5.
A kind of method of extracting ursolic acid from sea-buckthorn of the present invention has following beneficial effect compared with prior art: the present invention utilizes supercritical CO
2Extraction process extracts ursolic acid and Oleanolic Acid from seabuckthorn fruit peel, reach most optimum distribution of resources, improves the purpose of sea-buckthorn series products added value.Because ursolic acid and Oleanolic Acid are triterpenic acid class isomers, structural similitude, the present invention utilizes reversed-phased high performace liquid chromatographic that the two is separated.
Description of drawings
Fig. 1 is a kind of method process flow sheet that extracts ursolic acid from sea-buckthorn of the present invention.
Embodiment
Below in conjunction with embodiment a kind of method and technology scheme of extracting ursolic acid from sea-buckthorn of the present invention is further described.
A kind of method of extracting ursolic acid from sea-buckthorn of the present invention comprises the steps:
(1) after the pre-treatment of sea buckthorn fruit is the cleaning of sea buckthorn fruit process, centrifuging and taking juice, obtains the process of fruit juice, seed of Fructus Hippophae and seabuckthorn fruit peel;
(2) extraction of ursolic acid and Oleanolic Acid is that seabuckthorn fruit peel is through degreasing, supercritical CO
2Extraction, get supernatant liquor after centrifugal, measure the ursolic acid content of target product in the supernatant liquor, promptly get crude extract after the drying; Extraction conditions is: 25 ℃ of extraction temperature, extracting pressure 25MPa, carry agent (this carries agent is dehydrated alcohol) 100ml, ethanol volume fraction 90%, the target extract is that tartaric acid and Oleanolic Acid leaching yield are 288mg/100g;
(3) be to utilize reversed-phased high performace liquid chromatographic separating of ursolic acid and Oleanolic Acid, with the two separation.Concrete grammar is as follows: chromatographic column: Nucleosil C
18Post; Moving phase: 85: 15 methanol-water; Detect wavelength: 210nm; Flow velocity: 0.8ml/min; Column temperature: 25 ℃; Sample size: 20 μ l; External standard method quantitative analysis, ursolic acid and Oleanolic Acid theoretical tray number average greater than 10000, two component resolution greater than 1.5.
Described chromatographic column: Nucleosil C
18Post is that German Macherey-Nagel company produces 4.6mm * 250mm.
Embodiment 1.
(1) after the pre-treatment of sea buckthorn fruit is the cleaning of sea buckthorn fruit process, centrifuging and taking juice, obtains the process of fruit juice, seed of Fructus Hippophae and seabuckthorn fruit peel.
(2) extraction of ursolic acid and Oleanolic Acid is that seabuckthorn fruit peel is through degreasing, supercritical CO
2Extraction, get supernatant liquor after centrifugal, measure the content (in ursolic acid) of target product in the supernatant liquor, promptly get crude extract after the drying.Determine that extraction conditions is: 25 ℃ of extraction temperature, extracting pressure 25MPa, carry agent 100ml, ethanol volume fraction 90%, target extract leaching yield is 288mg/100g.
(3) be to utilize reversed-phased high performace liquid chromatographic separating of ursolic acid and Oleanolic Acid, with the two separation.Concrete grammar is as follows: chromatographic column: Nucleosil C
18Post (4.6mm * 250mm, German Macherey-Nagel company); Moving phase: methanol-water (85: 15); Detect wavelength: 210nm; Flow velocity: 0.8ml/min; Column temperature: 25 ℃; Sample size: 20 μ l.External standard method quantitative analysis, ursolic acid and Oleanolic Acid theoretical tray number average greater than 10000, two component resolution greater than 1.5.
Technical requirements
(1) ursolic acid sense organ requirement
| Project | Index |
| Color and luster | Color and luster is even, pistac |
| Smell | Has special characteristic odor |
| Outward appearance | The pistac powder, the visible impurity of no naked eyes, quality evenly do not have caking. |
(2) ursolic acid physics and chemistry requirement
| Project | Index |
| Ursolic acid (%) 〉= | ??20.0 |
| Solubleness (%) 〉= | ??95.0 |
| Granularity (order) 〉= | ??80 |
| Ash content (%)≤ | ??6.0 |
| Moisture (%)≤ | ??5.0 |
(3) Oleanolic Acid sense organ requirement
| Project | Index |
| Color and luster | Color and luster is even, white |
| Smell | Odorless, tasteless |
| Outward appearance | White powder, the visible impurity of no naked eyes, quality evenly do not have caking. |
(4) Oleanolic Acid physics and chemistry requirement
| Project | Index |
| Oleanolic Acid (%) 〉= | ??90.0 |
| Solubleness (%) 〉= | ??95.0 |
| Granularity (order) 〉= | ??80 |
| Ash content (%)≤ | ??6.0 |
| Moisture (%)≤ | ??5.0 |
(5) hygienic requirements
| Project | Index |
| Plumbous (in pb) mg/kg≤ | ??2.0 |
| Arsenic (in As) mg/kg | ??0.5 |
| Copper (in Cu) mg/kg | ??5.0 |
| Total number of bacterial colony (cfu/g)≤ | ??1000 |
| Coliform (MPN/100g) | ??30 |
| Mould, yeast (cfu/g)≤ | ??50 |
| Pathogenic bacterium (Salmonellas, Shigellae, streptococcus aureus, Hemolytic streptococcus) | Must not detect |
Claims (2)
1. method of extracting ursolic acid from sea-buckthorn, it is characterized in that: described method comprises the steps:
(1) after the pre-treatment of sea buckthorn fruit is the cleaning of sea buckthorn fruit process, centrifuging and taking juice, obtains the process of fruit juice, seed of Fructus Hippophae and seabuckthorn fruit peel;
(2) extraction of ursolic acid and Oleanolic Acid is that seabuckthorn fruit peel is through degreasing, supercritical CO
2Extraction, get supernatant liquor after centrifugal, measure the ursolic acid content of target product in the supernatant liquor, promptly get crude extract after the drying; Extraction conditions is: 25 ℃ of extraction temperature, extracting pressure 25MPa, carry agent 100ml, ethanol volume fraction 90%, target extract leaching yield is 288mg/100g.
(3) be to utilize reversed-phased high performace liquid chromatographic separating of ursolic acid and Oleanolic Acid, with the two separation.Concrete grammar is as follows: chromatographic column: Nucleosil C
18Post; Moving phase: 85: 15 methanol-water; Detect wavelength: 210nm; Flow velocity: 0.8ml/min; Column temperature: 25 ℃; Sample size: 20 μ l; External standard method quantitative analysis, ursolic acid and Oleanolic Acid theoretical tray number average greater than 10000, two component resolution greater than 1.5.
2. the method for extracting ursolic acid from sea-buckthorn according to claim 1 is characterized in that: described chromatographic column: Nucleosil C
18Post is that German Macherey-Nagel company produces 4.6mm * 250mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910216298A CN101817863A (en) | 2009-11-18 | 2009-11-18 | Method for extracting ursolic acid from sea-buckthorn |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910216298A CN101817863A (en) | 2009-11-18 | 2009-11-18 | Method for extracting ursolic acid from sea-buckthorn |
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| CN101817863A true CN101817863A (en) | 2010-09-01 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351939A (en) * | 2011-09-05 | 2012-02-15 | 曾超 | Method for preparing high-purity ursolic acid and oleanolic acid from ligustrum lucidum ait |
| CN102887935A (en) * | 2012-09-28 | 2013-01-23 | 南京泽朗农业发展有限公司 | Method for extracting suaveolic acid A |
| CN109111496A (en) * | 2018-10-23 | 2019-01-01 | 青海清华博众生物技术有限公司 | The method for extraction and purification of triterpenic acid and triterpenic acid and triterpenoid saponin and application in sea-buckthorn |
| CN109106733A (en) * | 2017-06-22 | 2019-01-01 | 陕西天奎生物医药科技有限公司 | A kind of composition for preventing and treating diabetes and/or vascular complication disease, drug or health care product and its application |
| CN110317239A (en) * | 2019-08-13 | 2019-10-11 | 南京津奇生物科技有限公司 | A kind of preparation method for extracting Corosolic acid from fructus hippophae |
| CN110559322A (en) * | 2018-06-06 | 2019-12-13 | 邹玮 | Sea-buckthorn compound hard capsule for treating depression and preventing anxiety depression and preparation method thereof |
-
2009
- 2009-11-18 CN CN200910216298A patent/CN101817863A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351939A (en) * | 2011-09-05 | 2012-02-15 | 曾超 | Method for preparing high-purity ursolic acid and oleanolic acid from ligustrum lucidum ait |
| CN102887935A (en) * | 2012-09-28 | 2013-01-23 | 南京泽朗农业发展有限公司 | Method for extracting suaveolic acid A |
| CN109106733A (en) * | 2017-06-22 | 2019-01-01 | 陕西天奎生物医药科技有限公司 | A kind of composition for preventing and treating diabetes and/or vascular complication disease, drug or health care product and its application |
| CN110559322A (en) * | 2018-06-06 | 2019-12-13 | 邹玮 | Sea-buckthorn compound hard capsule for treating depression and preventing anxiety depression and preparation method thereof |
| CN109111496A (en) * | 2018-10-23 | 2019-01-01 | 青海清华博众生物技术有限公司 | The method for extraction and purification of triterpenic acid and triterpenic acid and triterpenoid saponin and application in sea-buckthorn |
| CN110317239A (en) * | 2019-08-13 | 2019-10-11 | 南京津奇生物科技有限公司 | A kind of preparation method for extracting Corosolic acid from fructus hippophae |
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Application publication date: 20100901 |