CN102757472B - Method for purifying beta-sitosterol from cornel kernels - Google Patents
Method for purifying beta-sitosterol from cornel kernels Download PDFInfo
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- CN102757472B CN102757472B CN201210261572.6A CN201210261572A CN102757472B CN 102757472 B CN102757472 B CN 102757472B CN 201210261572 A CN201210261572 A CN 201210261572A CN 102757472 B CN102757472 B CN 102757472B
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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 Dogwood pit rapid batch extract the method for high-purity beta one Sitosterol.
Background technology
β mono-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 has obvious curative effect; Have and suppress the absorption of human body to cholesterol, promote the catabolism of cholesterol, the biochemistry that suppresses cholesterol synthesizes the effect that reduces cholesterol that waits; And β mono-Sitosterol can be for prevention and treatment coronary heart disease, the heart trouble of atherosclerosis class; There are stronger anti-inflammatory and antipyretic effect, are similar to hydrocortisone, through base Phenylbutazone and Asprin, and without these type of Side effects of pharmaceutical drugs; Skin is had to good perviousness, can reduce lipoprotein, strengthen the activity of lipase, defence erythema, suppresses skin inflammation, keeps skin surface moisture, promotes skin metabolism, prevents skin aging etc., also has the effects such as generating and nourishing hair.So can be used as skin-nourishing agent for a lot of makeup; And can make hair grow strength, easy fracture, does not reduce electrostatic effect, protection scalp, so β mono-Sitosterol has replaced cholesterol to be widely used in the production of the makeup such as hair conditioner, hair tonic perfume now; Current research shows that β mono-Sitosterol is a kind of high-quality, natural " protecting the liver, protect liver " activeconstituents, can stablize, repair liver plasma membrane, makes the life state of liver cell in a kind of health.Generally speaking, β mono-Sitosterol has 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 wide market outlook.
Domestic existing separation and purification β mono-Sitosterol technology exists that yield is low, cost is high mostly, and the problem such as β mono-Sitosterol purity low (only have 60% left and right, be difficult to reach more than 90%).And the present invention be take skunk bush fruit stone and is taken full advantage of the byproduct in Chinese medicine preparation process as raw material production β mono-Sitosterol, so raw material resources are abundant, low production cost relatively.And extraction process is simple, do not need special production unit, non-pollution discharge, so easy handling, environmental protection, is convenient to large-scale industrial production.So extracting β mono-Sitosterol from Dogwood pit, research and development have obvious economic worth and realistic meaning.
Summary of the invention
Main purpose of the present invention is to overcome deficiency of the prior art, and provide a kind of from skunk bush fruit stone rapid batch extract the method for high-purity beta one Sitosterol.
The present invention a kind of from Dogwood pit the method for purifying beta one Sitosterol, comprise the following steps:
1) skunk bush fruit stone is ground into 15～20 object particles;
2) 95% edible ethanol that the particle of pulverizing is added to 5 times of weight soaks 24 hours, filters, and then squeezes fuel-displaced;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in amalgamation liquid, then by the oil plant and concentration 25%(W/W removed after ethanol) Na0H solution by M/V=1: 1 mixes, and saponification 3 hours refluxes under 75 degree;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, by filtrate at 65 ℃ concentrating under reduced pressure to the l/1O of original volume;
5) in filtrate, add equal-volume ethyl acetate extraction filtrate 2～3 times, extraction liquid is merged, the HCl solution with 2% adjusts extraction liquid to neutral, with saturated sodium-chloride water solution, washes 2 times; In extraction liquid, add appropriate dried sodium sulfate powder, stir at normal temperatures, remove unnecessary moisture in extraction liquid;
6) cross extraction liquid, under reduced pressure, evaporate to dryness filter extraction liquid, dry under 30 degree conditions by the yellow paste substance making, and makes β mono-Sitosterol crude product;
7) β mono-Sitosterol crude product is mixed in mass ratio with crystal solution ethyl acetate at 1: 0.2, heated and stirred under 50～60 ℃ of conditions, fully dissolves β mono-Sitosterol crude product.；
8) under heat filtering, filter and remove insoluble impurity, standing crystallization is after 6～7 hours under room temperature for filtrate, and filtration drying obtains β mono-Sitosterol white needle-like crystals;
9) white needle-like crystals β step 8) being obtained and oil mystery: ethyl acetate=6: 1 crystal solution is mixed according to the ratio of 1: 4, under reflux conditions stirring heating, fully dissolves β mono-Sitosterol white needle-like crystals again;
10) under heat filtering, filter to remove insoluble impurity, filtrate is standing crystallization filtration drying after 6～7 hours under room temperature, makes.
Compared with prior art, the present invention is that from Dogwood pit, rapid batch extracts highly purified β mono-Sitosterol by technology such as saponification, extraction, fractional crystallizations.There is the advantages such as velocity of separation is fast, separation costs is low, yield is high and abundant raw material is easy to get.And the method makes full use of concocts remaining fruit stone waste material after Chinese medicine skunk bush, cost is low, yield is high, and the product purity of producing is high, and (purity > 98%, fusing point is 140 1 141 ℃), crystal habit good (white needle-like crystals), suitablely as β mono-Sitosterol standard substance and medical material, use.
Embodiment
Embodiment 1
A method for purifying beta one Sitosterol from Dogwood pit, comprises the following steps:
1) skunk bush fruit stone is ground into 15 object particles;
2) 95% edible ethanol that the particle of pulverizing is added to 5 times of weight soaks 24 hours, filters, and then squeezes fuel-displaced;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in amalgamation liquid, then by the oil plant and concentration 25%(W/W removed after ethanol) Na0H solution by M/V=1: 1 mixes, and saponification 3 hours refluxes under 75 degree;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, by filtrate at 65 ℃ concentrating under reduced pressure to the l/1O of original volume;
5) in filtrate, add equal-volume ethyl acetate extraction filtrate 2～3 times, extraction liquid is merged, the HCl solution with 2% adjusts extraction liquid to neutral, with saturated sodium-chloride water solution, washes 2 times; In extraction liquid, add appropriate dried sodium sulfate powder, stir at normal temperatures, remove unnecessary moisture in extraction liquid;
6) cross extraction liquid, under reduced pressure, evaporate to dryness filter extraction liquid, dry under 30 degree conditions by the yellow paste substance making, and makes β mono-Sitosterol crude product;
7) β mono-Sitosterol crude product is mixed in mass ratio with crystal solution ethyl acetate at 1: 0.2, heated and stirred under 50 ℃ of conditions, fully dissolves β mono-Sitosterol crude product.；
8) under heat filtering, filter and remove insoluble impurity, standing crystallization is after 6 hours under room temperature for filtrate, and filtration drying obtains β mono-Sitosterol white needle-like crystals;
9) white needle-like crystals β step 8) being obtained and oil mystery: ethyl acetate=6: 1 crystal solution is mixed according to the ratio of 1: 4, under reflux conditions stirring heating, fully dissolves β mono-Sitosterol white needle-like crystals again;
10) under heat filtering, filter to remove insoluble impurity, filtrate is standing crystallization filtration drying after 6 hours under room temperature, makes.
Embodiment 2
A method for purifying beta one Sitosterol from Dogwood pit, comprises the following steps:
1) skunk bush fruit stone is ground into 20 object particles;
2) 95% edible ethanol that the particle of pulverizing is added to 5 times of weight soaks 24 hours, filters, and then squeezes fuel-displaced;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in amalgamation liquid, then by the oil plant and concentration 25%(W/W removed after ethanol) Na0H solution by M/V=1: 1 mixes, and saponification 3 hours refluxes under 75 degree;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, by filtrate at 65 ℃ concentrating under reduced pressure to the l/10 of original volume;
5) in filtrate, add equal-volume ethyl acetate extraction filtrate 2～3 times, extraction liquid is merged, the HCl solution with 2% adjusts extraction liquid to neutral, with saturated sodium-chloride water solution, washes 2 times; In extraction liquid, add appropriate dried sodium sulfate powder, stir at normal temperatures, remove unnecessary moisture in extraction liquid;
6) cross extraction liquid, under reduced pressure, evaporate to dryness filter extraction liquid, dry under 30 degree conditions by the yellow paste substance making, and makes β mono-Sitosterol crude product;
7) β mono-Sitosterol crude product is mixed in mass ratio with crystal solution ethyl acetate at 1: 0.2, heated and stirred under 60 ℃ of conditions, fully dissolves β mono-Sitosterol crude product.；
8) under heat filtering, filter and remove insoluble impurity, standing crystallization is after 7 hours under room temperature for filtrate, and filtration drying obtains β mono-Sitosterol white needle-like crystals;
9) white needle-like crystals β step 8) being obtained and oil mystery: ethyl acetate=6: 1 crystal solution is mixed according to the ratio of 1: 4, under reflux conditions stirring heating, fully dissolves β mono-Sitosterol white needle-like crystals again;
10) under heat filtering, filter to remove insoluble impurity, filtrate is standing crystallization filtration drying after 7 hours under room temperature, makes.
Claims (1)
1. purify from the Dogwood pit method of β-sitosterol, is characterized in that comprising the following steps:
1) skunk bush fruit stone is ground into 15～20 object particles;
2) 95% edible ethanol that the particle of pulverizing is added to 5 times of weight soaks 24 hours, filters, and then squeezes fuel-displaced;
3) merging filtrate and pressed liquor, concentrating under reduced pressure is removed the ethanol in amalgamation liquid, then by the oil plant and concentration 25 %(W/W removed after ethanol) NaOH solution by M/ V=1: 1 mixes, and saponification 3 hours refluxes under 75 degree;
4) cooling step 3) reaction solution that makes, and be cooled to 0 degree, separate out residue, filter and remove saponification resultant, by filtrate at 65 ℃ concentrating under reduced pressure to l/10 of original volume;
5) in filtrate, add equal-volume ethyl acetate extraction filtrate 2～3 times, extraction liquid is merged, the HCl solution with 2% adjusts extraction liquid to neutral, with saturated sodium-chloride water solution, washes 2 times; In extraction liquid, add appropriate dried sodium sulfate powder, stir at normal temperatures, remove unnecessary moisture in extraction liquid;
6) filter extraction liquid, evaporate to dryness extraction liquid under reduced pressure, the yellow paste substance making is dry under 30 degree conditions, make β-sitosterol crude product;
7) β-sitosterol crude product is mixed in mass ratio with ethyl acetate at 1: 0.2, heated and stirred under 50～60 ℃ of conditions, fully dissolves β-sitosterol crude product;
8) under heat filtering, filter and remove insoluble impurity, standing crystallization is after 6～7 hours under room temperature for filtrate, and filtration drying obtains β-sitosterol white needle-like crystals;
9) β-sitosterol step 8) being obtained and sherwood oil: the solution of ethyl acetate (V/V)=6: 1 mixes in the ratio of 1: 4, under reflux conditions stirring heating, fully dissolves β-sitosterol white needle-like crystals again;
10) under heat filtering, filter to remove insoluble impurity, filtrate is standing crystallization filtration drying after 6～7 hours under room temperature, makes.
Priority Applications (1)
| 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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| CN102757472B true CN102757472B (en) | 2014-01-15 |
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| 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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| CN1724555A (en) * | 2005-07-06 | 2006-01-25 | 浙江大学 | Method for extracting and purifying beta-sitosterin from remnant of rapeseed oil |
| CN101434633B (en) * | 2008-12-22 | 2011-11-02 | 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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