CN101318985A - Preparation method for ursolic acid, produced products and application thereof - Google Patents
Preparation method for ursolic acid, produced products and application thereof Download PDFInfo
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- CN101318985A CN101318985A CNA2008103029400A CN200810302940A CN101318985A CN 101318985 A CN101318985 A CN 101318985A CN A2008103029400 A CNA2008103029400 A CN A2008103029400A CN 200810302940 A CN200810302940 A CN 200810302940A CN 101318985 A CN101318985 A CN 101318985A
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- ursolic acid
- ethanol
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Abstract
The invention discloses a method for preparing ursolic acid and a product and an application thereof. The method comprises the following steps that: loquat leaves are pulverized, added with 95 percent ethanol and subjected to ultrasonic extraction for 0.5 to 2 hours; an extractant is filtered by a micromembrane; a filtrate is separated by an ultrafiltration membrane and a nanofiltration membrane to produce a mixed solution of the ethanol and the ursolic acid; the ethanol is reclaimed, and the ursolic acid is obtained; the obtained ursolic acid is mixed with grosvener siraitia and honey to prepare grosvener siraitia honey cream. The invention adopts a method of combining ultrasonic extraction and membrane separation and purification, and extracts the ursolic acid from the loquat leaves; the method has relatively simple process flow, small loss of effective compositions, an ursolic acid yield of more than 75 percent, small ethanol amount and low energy consumption, thereby reducing extraction cost; and the prepared grosvener siraitia honey cream has the faint scent and sweetness of the grosvener siraitia and the light fragrance, fresh and sweet taste and mellowness of the honey, and has the functions of sedation, heat-clearing and lung-moistening, intestine moistening, defaecation and sleep improvement, thereby becoming a high-quality health-care product integrating nutrition and health care.
Description
(1) technical field:
The present invention relates to a kind of preparation method of ursolic acid and products thereof and use, belong to crude drug with extraction of active ingredients and applied technical field.
(2) background technology:
Loquat Leaf is the leaf of Rosaceae loquat platymiscium loquat, and contained main component has volatile oil, bitter benevolence glucoside, saponin, ursolic acid, Oleanolic Acid, VITMAIN B1 and c, tannin, organic acid etc.Ursolic acid (molecular formula: C wherein
30H
48O
3, molecular weight: 456.68) content in dry Loquat Leaf is about about 1%.Ursolic acid has various biological effects such as calmness, anti-inflammatory, antibiotic, anti-diabetic, antiulcer agent, lowering blood glucose.It has discovered in recent years carcinogenesis, anti-promoting, induces differentiation of F9 teratocarcinoma cell and blood vessel formation against function, very likely becomes low toxicity new type anticancer medicine efficiently.In addition, ursolic acid has tangible antioxygen function, thereby is widely used as medicine and cosmetic material.
At present, the method for extracting ursolic acid from Loquat Leaf has ultrasonic extraction and soxhlet extraction, and employed solvent is ethanol, alcohol reflux, concentrate and reclaim ethanol, condensed cream washes the final vacuum drying with water, and powder gets dry extract, dried cream powder is again with using activated carbon decolorizing behind the dissolve with ethanol, destainer goes to add elutriation behind the ethanol and goes out a large amount of precipitations, pH value is transferred to 2-2.5 carry out precipitate and separate, collecting precipitation thing, and be washed with water to neutrality, vacuum-drying obtains the crude extract that main component is a ursolic acid.
Aforesaid method extracts the technical process more complicated of ursolic acid, and the ethanol consumption is big, and three washings make loss of effective components big, and the yield of ursolic acid has only about 60%, and twice dry energy consumption is more, thereby has increased cost.
(3) summary of the invention:
Technical problem to be solved by this invention is: adopt supersound extraction and membrane sepn to purify the method that combines and extract ursolic acid from Loquat Leaf, its technical process is simple, ursolic acid yield height, and cost is low; And the ursolic acid that extraction obtains made complex health care product.
The present invention is achieved in that preparation method of ursolic acid is: Loquat Leaf pulverized, and the ethanol ultrasonic extraction of adding 95% 0.5～2 hour, extracting solution filters with mocromembrane, filtrate is used ultra-filtration membrane and nanofiltration membrane separation again, get the mixed solution of ethanol and ursolic acid, reclaim ethanol, promptly get ursolic acid.Described mocromembrane filters can remove robust fibre class impurity, and ultra-filtration membrane separates can remove macromolecular substance such as pectin, protein, and nanofiltration membrane separation can be further purified, the enrichment ursolic acid.
Wherein, Loquat Leaf is crushed to 15～20 orders.If granularity is too little, be not easy to follow-up filtration purifying; Granularity is too big, and then the extraction of effective constituent is complete inadequately.
Carry out screening experiment according to extraction effect, determine that consumption of ethanol is 5～10 times of Loquat Leaf weight.
The aperture of described mocromembrane is 0.22 micron; The molecular weight of ultra-filtration membrane is 5000～10000; The molecular weight of nanofiltration membrane is 800～2000.
Operating pressure when mocromembrane filters is 0.1～0.3MPa; Operating pressure when ultra-filtration membrane separates is 0.2～0.5MPa; Operating pressure during nanofiltration membrane separation is 0.5～2MPa.
Feed temperature when mocromembrane filtration, ultra-filtration membrane separation, nanofiltration membrane separation is 25～30 ℃.
The ursolic acid that the above preparation method of ursolic acid prepares.
Aforementioned ursolic acid has application in the healthcare products of calmness, clearing heat and moistening lung, ease constipation, defaecation, improvement sleep effect in preparation
Specifically, count by weight percentage, get 0.1～0.5% ursolic acid, 19.5～29.9% Momordica-Glycosides and 70～80% honey mix, and stir, and make Grosvenor Momordica honey cream.
Preferred scheme is: count by weight percentage, get 0.1% ursolic acid, 24.9% Momordica-Glycosides and 75% honey mix, and stir 25～30 minutes, make Grosvenor Momordica honey cream.When taking, can drink should honey cream being deployed into beverage.
Ursolic acid is a kind of triterpene compound that is present in the natural phant such as Loquat Leaf, has effects such as calmness, anti-inflammatory, antibiotic, anti-diabetic, antiulcer agent, lowering blood glucose.Momordica-Glycosides extracts from Grosvenor Momordica, contains 80% or more Momordica-Glycosides in the extract, also contains a large amount of amino acid, fructose, and vitamin b6 usp and mineral substance, soluble in water and do not have a precipitation.Because it is low that the sugariness of Momordica-Glycosides be 300 times of sugar and heat content, be that the diabetic subject stablizes and do not have fermentable perfect additive, also be the desirable substitute of artificial sweetening agent.The contained main component of honey has fructose, glucose, amino acid (aspartic acid, L-glutamic acid, leucine, Isoleucine, Methionin, Threonine, Xie Ansuan etc.), vitamin B group, vitamins C and several mineral materials etc.; Its flavor is sweet, and is flat, goes into lung, board, large intestine channel, bowl spares is arranged, moisturizes, the merit of pain relieving, detoxifcation, can be used for treating xeropulmonary cough, the dry constipation of intestines, gastralgia, nasosinusitis, aphtha, the burning hot wound of soup, separates rhizome of Chinese monkshood poison.Ursolic acid, Momordica-Glycosides and honey three are share, made Grosvenor Momordica honey cream not only has the simple and elegant fragrance of the delicate fragrance of Momordica-Glycosides, sweet thick sense and honey, mouthfeel is fresh and sweet, and is mellow aromatic, and has the effect of calmness, clearing heat and moistening lung, ease constipation, defaecation, improvement sleep.
Compared with prior art, the present invention adopts supersound extraction and membrane sepn to purify the method that combines and extract ursolic acid from Loquat Leaf, and its technical process is simple relatively, loss of effective components is few, and the yield of ursolic acid is more than 75%, and the ethanol consumption is few, energy consumption is low, thereby has reduced extraction cost.The simple and elegant fragrance that not only has the delicate fragrance of Momordica-Glycosides, sweet thick sense and honey with ursolic acid that the present invention extracted and Momordica-Glycosides, the made Grosvenor Momordica honey cream of honey, mouthfeel is fresh and sweet, mellow aromatic, and have the effect of calmness, clearing heat and moistening lung, ease constipation, defaecation, improvement sleep, be the high-quality healthcare products that integrate nutrition and health care.
(4) embodiment:
Embodiments of the invention 1: from Loquat Leaf, extract ursolic acid according to the following steps:
Get Loquat Leaf and be crushed to 15～20 orders for 10 kilograms, in the extractor of packing into, add 50 kilograms of 95% edible ethanols, supersound extraction 1.5 hours, the mocromembrane that extracting solution is supplied with 0.22 micron pore size with pump carries out filtering and impurity removing, and its operating pressure is 0.2MPa, and feed temperature is 28 ℃; It is that 5000～10000 ultra-filtration membrane carries out rough purification and separates that filter pump is supplied with molecular weight, and its operating pressure is 0.4MPa, and temperature is 28 ℃, removes the macromole part in the solution; It is that 800～2000 nanofiltration membrane is carried out purification separation that gained filtrate is supplied with molecular weight with pump again, and its operating pressure is 1.5MPa, and temperature is 28 ℃, the liquid that sees through nanofiltration membrane is the mixture of ethanol and ursolic acid, reclaim ethanol with vacuum, promptly get ursolic acid, its yield of giving money as a gift is 75%.
Embodiments of the invention 2: prepare ursolic acid according to the following steps:
Get Loquat Leaf and be crushed to 15～20 orders for 5 kilograms, add 50 kilograms of 95% ethanol, supersound extraction 0.5 hour, extracting solution carries out filtering and impurity removing with the mocromembrane of 0.22 micron pore size, and its operating pressure is 0.3MPa, and feed temperature is 25 ℃; Filtrate is that 5000～10000 ultra-filtration membrane carries out rough purification and separates with molecular weight, and its operating pressure is 0.2MPa, and temperature is 30 ℃, removes the macromole part in the solution; It is that 800～2000 nanofiltration membrane is carried out purification separation that gained filtrate is supplied with molecular weight with pump again, and its operating pressure is 0.5MPa, and temperature is 25 ℃, and the liquid that sees through nanofiltration membrane is the mixture of ethanol and ursolic acid, reclaims ethanol, promptly gets ursolic acid, yield 75%.
Embodiments of the invention 3: the preparation of Grosvenor Momordica honey cream: get Momordica-Glycosides 24.9 grams, honey 75 grams and embodiment 1 prepared ursolic acid 0.1 gram, mix, stir and made its mixing in 25～30 minutes, promptly get Grosvenor Momordica honey cream.
Embodiments of the invention 4: the preparation of Grosvenor Momordica honey cream: get Momordica-Glycosides 195 grams, honey 800 grams and embodiment 2 prepared ursolic acid 5 grams, mix, stir, promptly get Grosvenor Momordica honey cream.
More than used Momordica-Glycosides can buy from the market, also can from Grosvenor Momordica, extract preparation according to prior art.
Experimental example: embodiment 3 or embodiment 4 prepared Grosvenor Momordica honey cream are deployed into beverage, offer the drunk by people of different ages, sex, its result adds up as follows:
(1) 50-70 year drinking person totally 50 people, women 30 people wherein, the constipation state often appears in the male sex 20 people before drinking.Drink 350 milliliters every day, drink 40 people that have clear improvement after the week, women 27 people wherein, the male sex 13 people.
(2) 20-50 year drinking person totally 70 people, the male sex 40 people wherein, women 30 people have states such as insomnia, the heart be hot-tempered before drinking.Drink 350 milliliters every day, the week back state of drinking obviously alleviates 60 people, 56 people that improve of sleep wherein, and 54 people of the hot-tempered improvement of the heart, both all have 50 people of improvement.
Claims (10)
1. a preparation method of ursolic acid is characterized in that: Loquat Leaf is pulverized the ethanol ultrasonic extraction of adding 95% 0.5～2 hour, extracting solution filters with mocromembrane, and filtrate is used ultra-filtration membrane and nanofiltration membrane separation again, gets the mixed solution of ethanol and ursolic acid, reclaim ethanol, promptly get ursolic acid.
2. according to the described preparation method of ursolic acid of claim 1, it is characterized in that: Loquat Leaf is crushed to 15～20 orders.
3. according to the described preparation method of ursolic acid of claim 1, it is characterized in that: consumption of ethanol is 5～10 times of Loquat Leaf weight.
4. according to the described preparation method of ursolic acid of claim 1, it is characterized in that: the aperture of described mocromembrane is 0.22 micron; The molecular weight of ultra-filtration membrane is 5000～10000; The molecular weight of nanofiltration membrane is 800～2000.
5. according to claim 1 or 4 described preparation method of ursolic acid, it is characterized in that: the operating pressure when mocromembrane filters is 0.1～0.3MPa; Operating pressure when ultra-filtration membrane separates is 0.2～0.5MPa; Operating pressure during nanofiltration membrane separation is 0.5～2MPa.
6. according to claim 1 or 4 described preparation method of ursolic acid, it is characterized in that: the feed temperature when mocromembrane filtration, ultra-filtration membrane separation, nanofiltration membrane separation is 25～30 ℃.
7. the ursolic acid that each described preparation method of ursolic acid prepares among the claim 1-6.
8. the described ursolic acid of claim 7 has application in the healthcare products of calmness, clearing heat and moistening lung, ease constipation, defaecation, improvement sleep effect in preparation.
9. the application of described ursolic acid according to Claim 8 is characterized in that: count by weight percentage, get 0.1～0.5% ursolic acid, 19.5～29.9% Momordica-Glycosides and 70～80% honey mix, and stir, and make Grosvenor Momordica honey cream.
10. according to the application of the described ursolic acid of claim 9, it is characterized in that: count by weight percentage, get 0.1% ursolic acid, 24.9% Momordica-Glycosides and 75% honey mix, and stir 25～30 minutes, make Grosvenor Momordica honey cream.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008103029400A CN101318985A (en) | 2008-07-23 | 2008-07-23 | Preparation method for ursolic acid, produced products and application thereof |
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| CNA2008103029400A CN101318985A (en) | 2008-07-23 | 2008-07-23 | Preparation method for ursolic acid, produced products and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985459A (en) * | 2010-11-18 | 2011-03-16 | 桂林安和药业有限公司 | Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf |
| CN102318745A (en) * | 2011-10-10 | 2012-01-18 | 杭州银丰生物科技有限公司 | Method for preparing feed additive by extracting ursolic acid from loquat leaves |
| 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 |
| CN103923159A (en) * | 2014-04-24 | 2014-07-16 | 长沙麓园生物科技有限公司 | Method for extracting refined ursolic acid from loquat leaves |
| CN104688745A (en) * | 2010-05-20 | 2015-06-10 | 爱荷华大学研究基金会 | Methods for inhibiting muscle atrophy |
| US10159268B2 (en) | 2013-02-08 | 2018-12-25 | General Mills, Inc. | Reduced sodium food products |
-
2008
- 2008-07-23 CN CNA2008103029400A patent/CN101318985A/en active Pending
Cited By (9)
| 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 |
| CN104688745A (en) * | 2010-05-20 | 2015-06-10 | 爱荷华大学研究基金会 | Methods for inhibiting muscle atrophy |
| CN101985459A (en) * | 2010-11-18 | 2011-03-16 | 桂林安和药业有限公司 | Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf |
| CN101985459B (en) * | 2010-11-18 | 2012-11-28 | 桂林安和药业有限公司 | Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf |
| CN102318745A (en) * | 2011-10-10 | 2012-01-18 | 杭州银丰生物科技有限公司 | Method for preparing feed additive by extracting ursolic acid from loquat leaves |
| US10159268B2 (en) | 2013-02-08 | 2018-12-25 | General Mills, Inc. | Reduced sodium food products |
| US11540539B2 (en) | 2013-02-08 | 2023-01-03 | General Mills, Inc. | Reduced sodium food products |
| CN103923159A (en) * | 2014-04-24 | 2014-07-16 | 长沙麓园生物科技有限公司 | Method for extracting refined ursolic acid from loquat leaves |
| CN103923159B (en) * | 2014-04-24 | 2016-04-27 | 长沙麓园生物科技有限公司 | A kind of method of Hydrolysis kinetics ursolic acid from Loquat Leaf |
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Open date: 20081210 |