CN102757472A - Method for purifying beta-sitosterol from cornel kernels - Google Patents
Method for purifying beta-sitosterol from cornel kernels Download PDFInfo
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- CN102757472A CN102757472A CN2012102615726A CN201210261572A CN102757472A CN 102757472 A CN102757472 A CN 102757472A CN 2012102615726 A CN2012102615726 A CN 2012102615726A CN 201210261572 A CN201210261572 A CN 201210261572A CN 102757472 A CN102757472 A CN 102757472A
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Abstract
The invention relates to a method for separating and purifying a biological active substance phytosterin, particularly a method for quickly and massively extracting high-purity beta-sitosterol from cornel kernels. The high-purity beta-sitosterol is quickly and massively extracted from the cornel kernels by saponification, extraction, fractional crystallization and other techniques. The invention has the advantages of high separation speed, low separation cost, high yield, abundant and accessible raw material, and the like. By fully utilizing the residual kernel waste after processing the traditional Chinese medicine cornel, the method provided by the invention has the advantages of low cost, high yield, high product purity (the purity is higher than 98%, and the melting point is 140-141 DEG C) and favorable crystal shape (white acicular crystal); and the beta-sitosterol is suitable to be used as a sitosterol standard substance and medicinal raw material.
Description
Technical field:
The present invention relates to a kind of separation purification method of biologically active substance plant sterol, more particularly, relate to a kind of from skunk bush nuclear rapid batch extract the method for high-purity beta one Sitosterol.
Background technology
β one Sitosterol is the key intermediate that important steroid drugs and the raw materials for production of Vitamin D3 500,000 I.U/GM, particularly anti-sars (SARS) are total to medicine " glucocorticosteroid "; For cancer, for example treating cervical cancer and skin carcinoma all has tangible curative effect; Have the human body of inhibition to absorption of cholesterol, promote the catabolism of SUV, suppress the synthetic effect that waits reducing cholesterol of biochemistry of SUV; And β one Sitosterol can be used for prevention and treatment coronary heart disease, the heart trouble of atherosclerosis class; Stronger anti-inflammatory and antipyretic effect are arranged, be similar to HYDROCORTISONE INJECTIONS,, and do not have this type of Side effects of pharmaceutical drugs through basic Phenylbutazone and Asprin; Skin is had good perviousness, can reduce lipoprotein, strengthen the activity of lypase, the defence erythema suppresses skin inflammation, keeps skin surface moisture, promotes skin metabolism, prevents skin aging etc., also has effects such as generating and nourishing hair.Be used for a lot of makeup so can be used as the skin-nourishing agent; And can make hair grow strength, easy fracture does not reduce electrostatic effect, and the protection scalp is so β one Sitosterol has replaced cholesterol to be widely used in the production of makeup such as hair conditioner, hair tonic perfume now; Current research shows that β one Sitosterol is a kind of high-quality, natural " protecting the liver, protect liver " activeconstituents, can stablize, repair liver plasma membrane, makes liver cell be in a kind of healthy life state.Generally speaking, β one Sitosterol has the very big market potentiality, will become a kind of necessary goods and materials that are widely used in medicine, food and cosmetic industry, therefore has vast market prospect.
Domestic existing separation and purification β one Sitosterol technology exists mostly that yield is low, cost is high, and the low problems such as (have only about 60%, be difficult to reach more than 90%) of β one Sitosterol purity.And the present invention is that raw material production β one Sitosterol has made full use of the sub product in the Chinese medicine preparation process with the skunk bush fruit stone, so raw material resources are abundant, and relative low production cost.And extraction process is simple, does not need special production unit, non-pollution discharge, so easy handling, and large-scale industrial production is convenient in environmental protection.So research and development are extracted β one Sitosterol from skunk bush nuclear tangible economic worth and realistic meaning are arranged.
Summary of the invention
Main purpose of the present invention is to overcome deficiency of the prior art, and provide a kind of from the skunk bush fruit stone rapid batch extract the method for high-purity beta one Sitosterol.
The present invention a kind of from skunk bush nuclear the method for purifying beta one Sitosterol, may further comprise the steps:
1) the skunk bush fruit stone is ground into 15～20 purpose particles;
2) 95% edible ethanol that the particle of pulverizing is added 5 times of weight soaked 24 hours, filtered, and squeezed fuel-displaced then;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in the amalgamation liquid, and the Na0H solution that will remove oil plant and concentration 25% (W/W) behind the ethanol again is by M/V=1: 1 mixed, 75 degree refluxed saponification 3 hours;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, with filtrating at the l/1O of 65 ℃ of following concentrating under reduced pressure to original volume;
5) in filtrating, add equal-volume ethyl acetate extraction filtrating 2～3 times, extraction liquid is merged, the HCl solution with 2% transfers extraction liquid to neutral, washes 2 times with saturated sodium-chloride water solution; In extraction liquid, add an amount of dried sodium sulfate powder, stir at normal temperatures, remove redundant moisture in the extraction liquid;
6) cross extraction liquid, evaporate to dryness filter extraction liquid is dry under 30 degree conditions with the yellow paste substance that makes under reduced pressure, processes β one Sitosterol bullion;
7) β one Sitosterol bullion is mixed by mass ratio with crystal solution ETHYLE ACETATE at 1: 0.2, heated and stirred under 50～60 ℃ of conditions is fully dissolved β one Sitosterol bullion.；
8) heat filtering filters down and removes insoluble impurity, filtrates in leaving standstill crystallization under the room temperature after 6～7 hours, and filtration drying obtains β one Sitosterol white needle-like crystals;
9) the white needle-like crystals β and the oil mystery that step 8) are obtained: the crystal solution of ETHYLE ACETATE=6: 1 was according to 1: 4 mixed, and under refluxad stirring heating makes the fully dissolving once more of β one Sitosterol white needle-like crystals;
10) heat filtering filters down and removes insoluble impurity, filtrates and under room temperature, leaves standstill 6～7 hours after-filtration dryings of crystallization, makes.
Compared with prior art, the present invention is through technology such as saponification, extraction, fractional crystallizations, and rapid batch extracts highly purified β one Sitosterol in examining from skunk bush.Have advantages such as velocity of separation is fast, separation costs is low, yield is high and abundant raw material is easy to get.And this method makes full use of concocts the fruit stone waste material that is left after the Chinese medicine skunk bush; Cost is low; Yield is high; And the product purity of producing high (purity＞98%, fusing point are 140 1 141 ℃), crystal habit good (white needle-like crystals), suitable to β one Sitosterol standard substance and medical material use.
Embodiment
Embodiment 1
A kind of from skunk bush nuclear the method for purifying beta one Sitosterol, may further comprise the steps:
1) the skunk bush fruit stone is ground into 15 purpose particles;
2) 95% edible ethanol that the particle of pulverizing is added 5 times of weight soaked 24 hours, filtered, and squeezed fuel-displaced then;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in the amalgamation liquid, and the Na0H solution that will remove oil plant and concentration 25% (W/W) behind the ethanol again is by M/V=1: 1 mixed, 75 degree refluxed saponification 3 hours;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, with filtrating at the l/1O of 65 ℃ of following concentrating under reduced pressure to original volume;
5) in filtrating, add equal-volume ethyl acetate extraction filtrating 2～3 times, extraction liquid is merged, the HCl solution with 2% transfers extraction liquid to neutral, washes 2 times with saturated sodium-chloride water solution; In extraction liquid, add an amount of dried sodium sulfate powder, stir at normal temperatures, remove redundant moisture in the extraction liquid;
6) cross extraction liquid, evaporate to dryness filter extraction liquid is dry under 30 degree conditions with the yellow paste substance that makes under reduced pressure, processes β one Sitosterol bullion;
7) β one Sitosterol bullion is mixed by mass ratio with crystal solution ETHYLE ACETATE at 1: 0.2, heated and stirred under 50 ℃ of conditions is fully dissolved β one Sitosterol bullion.；
8) heat filtering filters down and removes insoluble impurity, filtrates in leaving standstill crystallization under the room temperature after 6 hours, and filtration drying obtains β one Sitosterol white needle-like crystals;
9) the white needle-like crystals β and the oil mystery that step 8) are obtained: the crystal solution of ETHYLE ACETATE=6: 1 was according to 1: 4 mixed, and under refluxad stirring heating makes the fully dissolving once more of β one Sitosterol white needle-like crystals;
10) heat filtering filters down and removes insoluble impurity, filtrates and under room temperature, leaves standstill 6 hours after-filtration dryings of crystallization, makes.
Embodiment 2
A kind of from skunk bush nuclear the method for purifying beta one Sitosterol, may further comprise the steps:
1) the skunk bush fruit stone is ground into 20 purpose particles;
2) 95% edible ethanol that the particle of pulverizing is added 5 times of weight soaked 24 hours, filtered, and squeezed fuel-displaced then;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in the amalgamation liquid, and the Na0H solution that will remove oil plant and concentration 25% (W/W) behind the ethanol again is by M/V=1: 1 mixed, 75 degree refluxed saponification 3 hours;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, with filtrating at the l/10 of 65 ℃ of following concentrating under reduced pressure to original volume;
5) in filtrating, add equal-volume ethyl acetate extraction filtrating 2～3 times, extraction liquid is merged, the HCl solution with 2% transfers extraction liquid to neutral, washes 2 times with saturated sodium-chloride water solution; In extraction liquid, add an amount of dried sodium sulfate powder, stir at normal temperatures, remove redundant moisture in the extraction liquid;
6) cross extraction liquid, evaporate to dryness filter extraction liquid is dry under 30 degree conditions with the yellow paste substance that makes under reduced pressure, processes β one Sitosterol bullion;
7) β one Sitosterol bullion is mixed by mass ratio with crystal solution ETHYLE ACETATE at 1: 0.2, heated and stirred under 60 ℃ of conditions is fully dissolved β one Sitosterol bullion.；
8) heat filtering filters down and removes insoluble impurity, filtrates in leaving standstill crystallization under the room temperature after 7 hours, and filtration drying obtains β one Sitosterol white needle-like crystals;
9) the white needle-like crystals β and the oil mystery that step 8) are obtained: the crystal solution of ETHYLE ACETATE=6: 1 was according to 1: 4 mixed, and under refluxad stirring heating makes the fully dissolving once more of β one Sitosterol white needle-like crystals;
10) heat filtering filters down and removes insoluble impurity, filtrates and under room temperature, leaves standstill 7 hours after-filtration dryings of crystallization, makes.
Claims (1)
1. the method for purifying beta one Sitosterol from skunk bush nuclear is characterized in that may further comprise the steps:
1) the skunk bush fruit stone is ground into 15～20 purpose particles;
2) 95% edible ethanol that the particle of pulverizing is added 5 times of weight soaked 24 hours, filtered, and squeezed fuel-displaced then;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in the amalgamation liquid, and the Na0H solution that will remove oil plant and concentration 25% (W/W) behind the ethanol again is by M/V=1: 1 mixed, 75 degree refluxed saponification 3 hours;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, with filtrating at the l/10 of 65 ℃ of following concentrating under reduced pressure to original volume;
5) in filtrating, add equal-volume ethyl acetate extraction filtrating 2～3 times, extraction liquid is merged, the HCl solution with 2% transfers extraction liquid to neutral, washes 2 times with saturated sodium-chloride water solution; In extraction liquid, add an amount of dried sodium sulfate powder, stir at normal temperatures, remove redundant moisture in the extraction liquid;
6) cross extraction liquid, evaporate to dryness filter extraction liquid is dry under 30 degree conditions with the yellow paste substance that makes under reduced pressure, processes β one Sitosterol bullion;
7) β one Sitosterol bullion is mixed by mass ratio with crystal solution ETHYLE ACETATE at 1: 0.2, heated and stirred under 50～60 ℃ of conditions is fully dissolved β one Sitosterol bullion.；
8) heat filtering filters down and removes insoluble impurity, filtrates in leaving standstill crystallization under the room temperature after 6～7 hours, and filtration drying obtains β one Sitosterol white needle-like crystals;
9) the white needle-like crystals β and the oil mystery that step 8) are obtained: the crystal solution of ETHYLE ACETATE=6: 1 was according to 1: 4 mixed, and under refluxad stirring heating makes the fully dissolving once more of β one Sitosterol white needle-like crystals;
10) heat filtering filters down and removes insoluble impurity, filtrates and under room temperature, leaves standstill 6～7 hours after-filtration dryings of crystallization, makes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210261572.6A CN102757472B (en) | 2012-07-26 | 2012-07-26 | Method for purifying beta-sitosterol from cornel kernels |
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| CN201210261572.6A CN102757472B (en) | 2012-07-26 | 2012-07-26 | Method for purifying beta-sitosterol from cornel kernels |
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| CN102757472A true CN102757472A (en) | 2012-10-31 |
| CN102757472B CN102757472B (en) | 2014-01-15 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478758A (en) * | 2016-10-08 | 2017-03-08 | 佛山市聚成生化技术研发有限公司 | The extraction process of Sitosterolum and its application in a kind of Moringa |
| CN106632567A (en) * | 2016-11-17 | 2017-05-10 | 青海泰柏特生物科技有限公司 | Method for extracting enriched phytosterol from quinoa bran |
| CN111778129A (en) * | 2020-06-17 | 2020-10-16 | 方国胜 | Nucleic acid and amino acid health oral liquid and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724555A (en) * | 2005-07-06 | 2006-01-25 | 浙江大学 | Method for extracting and purifying beta-sitosterin from remnant of rapeseed oil |
| CN101434633A (en) * | 2008-12-22 | 2009-05-20 | 西安蓝天生物工程有限责任公司 | Production method of high-content beta-sitosterin |
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- 2012-07-26 CN CN201210261572.6A patent/CN102757472B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724555A (en) * | 2005-07-06 | 2006-01-25 | 浙江大学 | Method for extracting and purifying beta-sitosterin from remnant of rapeseed oil |
| CN101434633A (en) * | 2008-12-22 | 2009-05-20 | 西安蓝天生物工程有限责任公司 | Production method of high-content beta-sitosterin |
Non-Patent Citations (2)
| Title |
|---|
| 尚遂存 等: "山茱萸果实成分研究", 《中药材》, vol. 12, no. 4, 30 April 1989 (1989-04-30), pages 29 - 32 * |
| 崔晓秋: "吴茱萸化学成分研究", 《中国优秀硕士学位论文全文数据库（电子期刊）医药卫生科技辑》, no. 4, 31 December 2004 (2004-12-31), pages 057 - 42 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478758A (en) * | 2016-10-08 | 2017-03-08 | 佛山市聚成生化技术研发有限公司 | The extraction process of Sitosterolum and its application in a kind of Moringa |
| CN106632567A (en) * | 2016-11-17 | 2017-05-10 | 青海泰柏特生物科技有限公司 | Method for extracting enriched phytosterol from quinoa bran |
| CN111778129A (en) * | 2020-06-17 | 2020-10-16 | 方国胜 | Nucleic acid and amino acid health oral liquid and preparation method thereof |
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| CN102757472B (en) | 2014-01-15 |
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