CN104788515B - Method for preparing high-purity water-soluble oleuropein by reduced pressure ultrasonic-assisted extraction - Google Patents
Method for preparing high-purity water-soluble oleuropein by reduced pressure ultrasonic-assisted extraction Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Abstract
The invention discloses a method for preparing high-purity water-soluble oleuropein by reduced pressure ultrasonic-assisted extraction, which belongs to the technical field of natural medicine extraction and preparation and comprises the following steps: the method comprises the steps of pretreatment of medicinal materials, ultrasonic extraction under reduced pressure, extraction-back extraction, decolorization, crystallization-recrystallization. The invention provides a novel process for preparing oleuropein with high purity and good water solubility by utilizing vacuum degree generated by decompression and cavitation effect and stirring effect generated by ultrasonic waves and adding a certain amount of extracting solution according to the characteristics of low melting point, easy decomposition and the like of the oleuropein through a simple separation and purification process. The product prepared by the process has the content of more than 95 percent, has the advantages of high product yield, simple process, mild separation and purification conditions, low toxicity, low production cost and the like, and is suitable for industrial production.
Description
Technical Field
The invention relates to a method for extracting and preparing high-purity water-soluble oleuropein, in particular to a method for extracting and preparing oleuropein under the assistance of reduced pressure and ultrasound.
Background
The folium Canarii albi is leaf of Olea europaea (Oleaeuropagaeal) of Olea of Oleaceae, and mainly contains secoiridoid and its glycoside, flavone and its glycoside, biflavone and its glycoside, and low molecular tannin. The main component of the olive leaf extract is iridoid bitter substances, and the Oleuropein (Oleuropein) with the highest activity is used. Oleuropein has a molecular weight of 540.5, CAS number: 32619-42-4.
Oleuropein is a phenol and flavonoid substance with a bimolecular structure, has a melting point of 87-89 ℃, is easy to absorb moisture, and can be decomposed when exposed to air and sunlight. The health-care tea has the important health-care functions of resisting oxidation, resisting tumors, delaying senility, enhancing cardiovascular function, treating chronic prostatitis, enhancing immunity, regulating endocrine system, protecting liver, resisting inflammation and the like, has the pharmacological actions of reducing blood fat and blood sugar, and is widely applied to important fields of food, cosmetics, biopharmaceuticals and the like.
Oleuropein has strong antibacterial and antiviral properties, and can be used for preparing medicine for treating diseases caused by virus, bacteria, protozoa, parasite and blood fluke, and treating common cold. Oleuropein can also protect skin cells from being damaged by ultraviolet rays, prevent ultraviolet rays from decomposing skin membrane lipids, promote fibroblasts to generate collagen, reduce the secretion of collagenase of the fibroblasts and resist glycan reaction of tissue cell membranes, thereby highly protecting the fibroblasts, naturally resisting the skin damage caused by oxidation, preventing the skin from being damaged by the ultraviolet rays, effectively maintaining the skin tenderness and elasticity and achieving the effects of protecting and tendering the skin. At present, oleuropein with high water solubility and 90 percent of content is mainly used in skin care products, can protect skin cells from being damaged by ultraviolet rays, effectively maintains the skin to be tender and elastic, and achieves the effects of strengthening and tendering the skin.
The extraction, separation and purification technology of the oleuropein is disclosed at present, generally, an alcohol extraction method or an alkali extraction method is adopted to extract effective components in olive leaves, and then a series of separation and purification steps such as column chromatography and the like are carried out to obtain the high-purity oleuropein, but in the traditional process, resin adsorption or filter membrane purification is required to be used for further improving the product content, so that the energy consumption is high, the material consumption is high, the time consumption is long, the product yield is low, and the industrial pollution is high; and due to the characteristics of low melting point, easy decomposition and the like, the general thermal extraction method is often decomposed in the extraction process, and finally the yield is low. Thus, the use of a single extraction method has certain disadvantages.
Patent CN102532217A discloses a method for extracting and separating high-content oleuropein from olive leaves, which comprises the following steps: cutting folium Canarii albi, extracting at low temperature, filtering, concentrating or directly performing chromatography, concentrating at low temperature, and drying to obtain oleuropein product with content of more than 80%. The method takes ethanol or water with certain concentration as an extraction solvent for low-temperature extraction, utilizes a resin series connection or secondary adsorption chromatography technology to greatly improve the content of the product, but the resin needs to be regenerated or reused, so that the post treatment is more complicated, the cost of the process is increased, and the expanded production cannot be realized. Patent CN102702287A discloses a method for extracting and purifying oleuropein from olive leaves, which comprises the following steps: extracting folium Canarii albi with alkaline solution of pH 8-10 at room temperature, subjecting the obtained extractive solution to molecular sieve type macroporous adsorbent resin column chromatography, eluting the column with 50-80% ethanol, collecting eluate containing target components, concentrating, and drying to obtain low-content oleuropein; dissolving low-content oleuropein in polar solvent with polarity value of 3.8-4.2, vacuum filtering, and concentrating the filtrate to obtain concentrated solution; adding organic solvent into the concentrated solution to adjust polarity, standing at low temperature to precipitate crystal, and drying to obtain high purity oleuropein. The process adopts alkaline solution for extraction, so that oleuropein can be hydrolyzed into hydroxytyrosol, the extraction time is long, the hydrolysis degree is high, and the yield of the product is low and is only about 4 percent. The application of the macroporous adsorption resin column can increase energy consumption and improve production cost. Patent CN101003557A discloses a preparation method of "olive leaf extract rich in high-purity oleuropein", which comprises the following steps: firstly, extracting olive leaves by using a polar solvent, then carrying out alkaline centrifugal sedimentation to obtain centrifugal clear liquid and precipitates, then carrying out membrane coupling separation to obtain concentrated solution passing through a nanofiltration membrane, then carrying out medium adsorption, eluting an adsorption medium to obtain eluent, carrying out vacuum concentration, and then carrying out vacuum freeze drying or spray drying to obtain the olive leaf extract which contains more than 50% of oleuropein and is rich in high-purity oleuropein. The process saves energy, is clean and environment-friendly, has more complicated steps, needs membrane separation and medium adsorption technologies, has higher cost and is not easy to realize industrial production. Patent CN102850416A discloses a method for preparing olive leaf extract and a device used by the method, which comprises the following steps: firstly, olive leaves are subjected to ultrasonic reduced pressure boiling extraction by using a mixed solvent, and vacuum filtration to obtain a clear solution; then petroleum ether is extracted to remove fat-soluble impurities and collect the lower clear liquid, the lower clear liquid is evaporated by rotation until the solvent has no alcohol smell, then diluted, the diluted liquid is purified by macroporous resin, the diluted liquid is kept stand for a period of time to ensure that oleuropein and flavonoid substances are fully adsorbed, then the oleuropein is eluted by using an ethanol-water mixed solvent with proper concentration and the target liquid is collected, the collected target liquid is purified by sephadex, the diluted liquid is kept stand and eluted by ethanol-water solution, then the eluent containing effective components is collected, the eluent is evaporated by rotation until no alcohol smell exists, and finally the extract is dried or obtained, wherein the oleuropein content is 85-92 percent larger and the total flavone content reaches 25-35 percent. The process has the disadvantages of complex purification steps, high material consumption and high energy consumption, and cannot realize good economic benefit. Patent CN102228514A discloses "a method for extracting oleuropein from olive leaves", which comprises: after the extraction with water or alcohol-water mixed solvent, the extract is concentrated and then sequentially subjected to three steps of separation: macroporous resin adsorption, alcohol-water solvent elution, decolorizing resin adsorption (decolorizing resin with good adsorption effect on pigment in olive extract (macroporous resin with good adsorption effect on oleuropein, eluting to remove other impurities) and organic solvent extraction, gradually separating and purifying oleuropein in the extract to obtain high-content oleuropein extract with oleuropein content higher than 40%. The process is simple and easy to operate, but the product content is low, the product cannot be directly added into medicines or cosmetics, and further separation and purification are needed.
Aiming at the defects of the production process, the invention emphatically solves the problems of low oleuropein extraction rate and easy decomposition, combines a simple and effective separation and purification process, develops a new process for quickly and efficiently extracting and preparing high-content oleuropein with good water solubility, has short production period, high extraction efficiency and simple and convenient separation and purification process, can realize green and environmental protection, reduces the production cost, improves the yield and quality of products, and is easy for industrial production.
Disclosure of Invention
The invention firstly provides the method for preparing the pure oleuropein product with high purity and good water solubility by combining the cavitation effect and the secondary effect of ultrasonic waves with a pressure reduction technology, adopting a compound extracting solution and adopting a simple and efficient separation and purification process. The technology can effectively prevent oleuropein from decomposing, improve the product yield and the purity, and has the characteristics of simple operation, high efficiency, environmental protection, low cost, easy expanded production and the like.
In order to solve the technical problems, the invention adopts the following technical scheme:
1) pretreatment of raw materials: cleaning olive leaves, drying in the sun, crushing, and sieving with a 80-mesh sieve to obtain olive leaf powder for later use;
2) and (3) carrying out reduced pressure ultrasonic extraction: soaking the olive leaf powder and the compound extracting solution for 12-24 hours according to the mass volume ratio of 1 g: 10-15mL, and carrying out ultrasonic extraction for 30-50 minutes under the conditions of the vacuum degree of 0.08-0.1MPa, the power of 200 and 240W and the temperature of 35-40 ℃ for twice; and (5) carrying out suction filtration to obtain a filtrate.
3) Extraction-back extraction: concentrating the extracting solution obtained in the step 2) under reduced pressure until the Baume degree is between 8 and 10, extracting for 3 to 4 times by using ethyl acetate, combining the extracting solutions, concentrating under reduced pressure until no ethyl acetate exists, performing back extraction by using ethyl ether, and further removing impurities; drying the extractum after back extraction under reduced pressure to obtain oleuropein crude product;
4) and (3) decoloring: ultrasonically dissolving the oleuropein crude product obtained in the step 3) with an alcohol solution with a certain concentration, performing suction filtration to obtain a clear solution, and adding a proper amount of active carbon for heating, refluxing and decoloring;
5) crystallization-recrystallization: concentrating the decolorized solution obtained in the step 4) under reduced pressure until the Baume degree is 8-10, dissolving with alcohol with a certain concentration, concentrating the alcohol solution under reduced pressure until no alcohol smell exists, drying, hot-dissolving with ethyl acetate, filtering while hot, standing at low temperature, filtering after crystal is separated out, collecting crystal, hot-dissolving the crystal with ethyl acetate, and recrystallizing according to the steps to obtain pure oleuropein with good water solubility and high content.
Specifically, the compound extracting solution in the step 2) is a mixed solution of 95% ethanol and 95% methanol according to the volume ratio of 1: 1.
Specifically, the suction filtration conditions in the step 2) are as follows: the vacuum degree is 0.07-0.09 MPa.
Specifically, the conditions of the reduced pressure concentration in the step 3) are as follows: the vacuum degree is 0.07-0.09MPa, and the temperature is 40-50 ℃.
Specifically, the total volume ratio of the concentrated solution and the ethyl acetate in the step 3) is 1: 15-20.
Specifically, the mass volume ratio of the concentrated extract to the ether in the step 3) is 1: 5-10.
Specifically, the reduced-pressure drying conditions in the step 3) are as follows: the vacuum degree is 0.09-0.1MPa, and the temperature is 35-40 ℃.
Specifically, the alcoholic solution with a certain concentration in the step 3) is: 10-30% ethanol or methanol solution.
Specifically, the conditions of the heating reflux decoloring treatment in the step 4) are as follows: the addition amount of the active carbon is 2-3 per mill of the weight of the active carbon, and the temperature is 45-50 ℃.
Specifically, the conditions of the reduced pressure concentration in the step 5) are as follows: the vacuum degree is 0.09-0.1MPa, and the temperature is 45-50 ℃.
Specifically, the alcoholic solution with a certain concentration in the step 3) is: 95% ethanol or methanol solution.
Specifically, the conditions for hot-dissolving ethyl acetate in the step 5) are as follows: the mass volume ratio of the oleuropein crude product to the ethyl acetate is 1 g: 8-10mL, and the hot melting temperature is 45-50 ℃.
Specifically, the low-temperature standing condition in the step 5) is as follows: the low temperature is 0-5 ℃, and the standing time is 12-24 hours.
Detailed description of the invention
[ example 1 ]
Taking 1kg of olive leaves, cleaning, airing, crushing, sieving with a 80-mesh sieve, adding 10L of compound extracting solution (95% ethanol and 95% methanol in a volume ratio of 1: 1), and soaking for 12 h. Performing reduced pressure ultrasonic extraction for 30 minutes by using reduced pressure ultrasonic extraction equipment under the conditions of vacuum degree of 0.08MPa, power of 200W and temperature of 35 ℃, extracting twice, performing suction filtration under the vacuum degree of 0.07MPa, and combining filtrates of the two times. Concentrating the filtrate under reduced pressure at 40 deg.C under vacuum degree of 0.07MPa to Baume degree of 8. Extracting the concentrated solution with 3L ethyl acetate for three times, collecting ethyl acetate extractive solution, concentrating under reduced pressure until no ethyl acetate exists, performing back extraction with 0.3L diethyl ether for three times to remove impurities, recovering diethyl ether extractive phase, and drying the residual phase under reduced pressure to obtain oleuropein crude product. And ultrasonically dissolving the dried crude product by using 0.15L of 10% ethanol solution, performing suction filtration to obtain a clear solution, and then adding 0.8g of activated carbon for heating, refluxing and decoloring. Concentrating the decolorized solution under reduced pressure until the Baume degree is 8, dissolving with 0.1L 95% ethanol, concentrating the ethanol solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with 0.1L ethyl acetate at 45 deg.C, filtering while hot, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with 0.07L ethyl acetate at 45 deg.C, and recrystallizing according to the above steps to obtain pure oleuropein product with good water solubility and high content, with purity of 95.06% and yield of 6.86%.
[ example 2 ]
Taking 5kg of olive leaves, cleaning, airing, crushing, sieving with a 80-mesh sieve, adding 60L of the compound extracting solution, and soaking for 15 h. Performing reduced pressure ultrasonic extraction for 40 minutes by using reduced pressure ultrasonic extraction equipment under the conditions of vacuum degree of 0.08MPa, power of 220W and temperature of 40 ℃, extracting twice, performing suction filtration under the vacuum degree of 0.07MPa, and combining filtrates of the two times. Concentrating the filtrate under reduced pressure at 40 deg.C under vacuum degree of 0.07MPa to Baume degree of 8. Extracting the concentrated solution with 15L ethyl acetate for three times, collecting ethyl acetate extractive solution, concentrating under reduced pressure until no ethyl acetate exists, performing back extraction with 1L diethyl ether for three times to remove impurities, recovering diethyl ether extract phase, and drying the raffinate phase under reduced pressure to obtain oleuropein crude product. And ultrasonically dissolving the dried crude product by using 0.8L of 10% ethanol solution, performing suction filtration to obtain a clear solution, and then adding 5g of activated carbon for heating, refluxing and decoloring. Concentrating the decolorized solution under reduced pressure until the Baume degree is 8, dissolving with 0.5L 95% ethanol, concentrating the ethanol solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with 0.5L ethyl acetate at 45 deg.C, filtering while hot, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with 0.35L ethyl acetate at 45 deg.C, and recrystallizing according to the above steps to obtain pure oleuropein product with good water solubility and high content, with purity of 95.34% and yield of 7.03%.
[ example 3 ]
Taking 10kg of olive leaves, cleaning, airing, crushing, sieving with a 80-mesh sieve, adding 130L of the compound extracting solution, and soaking for 18 h. Performing reduced pressure ultrasonic extraction for 50 minutes by using reduced pressure ultrasonic extraction equipment under the conditions of vacuum degree of 0.08MPa, power of 240W and temperature of 40 ℃, extracting twice, and performing suction filtration and combination on filtrate obtained by the two times under the vacuum degree of 0.07 MPa. Concentrating the filtrate under reduced pressure at 40 deg.C under vacuum degree of 0.07MPa to Baume degree of 8. Extracting the concentrated solution with 30L ethyl acetate for three times, collecting ethyl acetate extractive solution, concentrating under reduced pressure until no ethyl acetate exists, performing back extraction with 2L diethyl ether for three times to remove impurities, recovering diethyl ether extractive phase, and drying the residual phase under reduced pressure to obtain oleuropein crude product. And ultrasonically dissolving the dried crude product by using 1.6L of 10% ethanol solution, performing suction filtration to obtain a clear solution, and adding 11g of activated carbon for heating reflux decoloring. Concentrating the decolorized solution under reduced pressure until the Baume degree is 8, dissolving with 0.5L 95% ethanol, concentrating the alcoholic solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with 0.8L ethyl acetate at 45 deg.C, filtering while hot, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with 0.7L ethyl acetate at 45 deg.C, and recrystallizing according to the above steps to obtain pure oleuropein product with good water solubility and high content, wherein the purity can reach 95.62%, and the yield is 7.41%.
[ example 4 ]
Taking 100kg of olive leaves, cleaning, airing, crushing, sieving with a 80-mesh sieve, adding 1500L of the compound extracting solution, and soaking for 20 h. Performing reduced pressure ultrasonic extraction for 50 minutes by using reduced pressure ultrasonic extraction equipment under the conditions of vacuum degree of 0.08MPa, power of 240W and temperature of 40 ℃, extracting twice, performing suction filtration and combination on filtrate obtained in two times under the vacuum degree of 0.07MPa, and concentrating the filtrate under reduced pressure under the conditions of vacuum degree of 0.07MPa and temperature of 40 ℃ until the Baume degree is 8. Extracting the concentrated solution with 300L ethyl acetate for three times, collecting ethyl acetate extractive solution, concentrating under reduced pressure until no ethyl acetate exists, back-extracting with 21L diethyl ether for three times to remove impurities, recovering diethyl ether extractive phase, and oven drying the residual phase under reduced pressure to obtain oleuropein crude product. And ultrasonically dissolving the dried crude product by using 17L of 10% ethanol solution, performing suction filtration to obtain a clear solution, and then adding 120g of activated carbon for heating reflux decoloring treatment. Concentrating the decolorized solution under reduced pressure until the Baume degree is 8, dissolving with 5L 95% ethanol, concentrating the alcoholic solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with 9L ethyl acetate at 45 deg.C, filtering, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with 8L ethyl acetate at 45 deg.C, and recrystallizing according to the above steps to obtain pure oleuropein with good water solubility and high content, with purity of 95.83% and yield of 7.49%.
[ example 5 ]
Taking 300kg of olive leaves, cleaning, airing, crushing, sieving with a 80-mesh sieve, adding 4500L of compound extracting solution, and soaking for 24 h. Performing reduced pressure ultrasonic extraction for 50 minutes by using reduced pressure ultrasonic extraction equipment under the conditions of vacuum degree of 0.08MPa, power of 240W and temperature of 40 ℃, extracting twice, and performing suction filtration and combination on filtrate obtained by the two times under the vacuum degree of 0.07 MPa. Concentrating the filtrate under reduced pressure at 40 deg.C under vacuum degree of 0.07MPa to Baume degree of 8. Extracting 900L ethyl acetate for three times to obtain concentrated solution, collecting ethyl acetate extractive solution, concentrating under reduced pressure until no ethyl acetate exists, performing back extraction with 60L diethyl ether for three times to remove impurities, recovering diethyl ether extractive phase, and drying under reduced pressure to obtain oleuropein crude product. And ultrasonically dissolving the dried crude product by using 50L of 10% ethanol solution, performing suction filtration to obtain a clear solution, and then adding 360g of activated carbon for heating reflux decoloring treatment. Concentrating the decolorized solution under reduced pressure until the Baume degree is 8, dissolving with 15L 95% ethanol, concentrating the ethanol solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with 27L ethyl acetate at 45 deg.C, filtering, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with 25L ethyl acetate at 45 deg.C, and recrystallizing according to the above steps to obtain pure oleuropein with good water solubility and high content, wherein the purity can reach 95.90%, and the yield is 7.51%.
[ example 6 ]
Taking 500kg of olive leaves, cleaning, airing, crushing, sieving with a 80-mesh sieve, adding 7500L of compound extracting solution, and soaking for 24 h. Performing reduced pressure ultrasonic extraction for 50 minutes by using reduced pressure ultrasonic extraction equipment under the conditions of vacuum degree of 0.08MPa, power of 240W and temperature of 40 ℃, extracting twice, and performing suction filtration and combination on filtrate obtained by the two times under the vacuum degree of 0.07 MPa. Concentrating the filtrate under reduced pressure at 40 deg.C under vacuum degree of 0.07MPa to Baume degree of 8. Taking 1500L ethyl acetate to carry out back extraction on concentrated solution for three times, collecting ethyl acetate extract, concentrating under reduced pressure until no ethyl acetate exists, extracting with 102L diethyl ether for three times to remove impurities, recovering diethyl ether extract phase, and drying under reduced pressure extraction residual phase to obtain oleuropein crude product. And ultrasonically dissolving the dried crude product by using 75L 10% ethanol solution, performing suction filtration to obtain a clear solution, and then adding 600g of activated carbon for heating reflux decoloring treatment. Concentrating the decolorized solution under reduced pressure until the Baume degree is 8, dissolving with 25L 95% ethanol, concentrating the alcoholic solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with 44L ethyl acetate at 45 deg.C, filtering, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with 41L ethyl acetate at 45 deg.C, and recrystallizing according to the above steps to obtain pure oleuropein with good water solubility and high content, wherein the purity can reach 95.98%, and the yield is 7.50%.
Claims (9)
1. A method for preparing oleuropein by decompression ultrasonic coupling extraction is characterized by comprising the following steps:
1) pretreating medicinal materials: cleaning olive leaves, drying in the sun, crushing, and sieving with a 80-mesh sieve to obtain olive leaf powder for later use;
2) and (3) carrying out reduced pressure ultrasonic extraction: soaking the olive leaf powder and the extracting solution for 12-24 hours according to the mass-volume ratio of 1 g: 10-15mL, and carrying out ultrasonic extraction for 30-50 minutes under the conditions of the vacuum degree of 0.08-0.1MPa, the power of 200 and 240W and the temperature of 35-40 ℃ for twice; filtering to obtain filtrate;
3) extraction-back extraction: concentrating the extracting solution obtained in the step 2) under reduced pressure until the Baume degree is between 8 and 10, extracting for 3 to 4 times by using ethyl acetate, combining the extracting solutions, concentrating under reduced pressure until no ethyl acetate exists, performing back extraction by using ethyl ether, and further removing impurities; drying the extractum after back extraction under reduced pressure to obtain oleuropein crude product;
4) and (3) decoloring: ultrasonically dissolving the oleuropein crude product obtained in the step 3) with an alcohol solution with a certain concentration, performing suction filtration to obtain a clear solution, and adding a proper amount of active carbon for heating, refluxing and decoloring;
5) crystallization-recrystallization: concentrating the decolorized solution obtained in step 4) under reduced pressure until the Baume degree is 8-10, dissolving with alcoholic solution with certain concentration, concentrating the alcoholic solution under reduced pressure until no alcohol smell exists, oven drying, dissolving with ethyl acetate, filtering while hot, standing at low temperature, filtering to collect crystals after crystals are separated out, dissolving the crystals with ethyl acetate, recrystallizing according to the above steps to obtain oleuropein;
the special extractant in the step 2) is a compound solution of 95 percent ethanol and 95 percent methanol according to the volume ratio of 1: 1;
the reduced pressure concentration condition in the step 3) is as follows: the vacuum degree is 0.07-0.09MPa, and the temperature is 40-50 ℃.
2. The method according to claim 1, wherein the suction filtration in step 2) is performed under the following conditions: the vacuum degree is 0.07-0.09 MPa.
3. The method according to claim 1, wherein the total volume ratio of the concentrated solution to the ethyl acetate in the step 3) is 1: 15-20.
4. The method as claimed in claim 1, wherein the concentration under reduced pressure in step 3) is carried out until the mass-to-volume ratio of the ethyl acetate extract without ethyl acetate to the diethyl ether is 1: 5-10.
5. The method as claimed in claim 1, wherein the reduced pressure drying in step 3) is performed under the following conditions: the vacuum degree is 0.09-0.1MPa, and the temperature is 35-40 ℃.
6. The method according to claim 1, wherein the conditions of the heating reflux decoloring treatment in the step 4) are as follows: the adding amount of the active carbon is 2-3 per mill of the weight of the active carbon, and the temperature is 45-50 ℃.
7. The method according to claim 1, wherein the reduced pressure concentration in step 5) is performed under the following conditions: the vacuum degree is 0.09-0.1MPa, and the temperature is 45-50 ℃.
8. The method according to claim 1, wherein the conditions for hot-dissolving ethyl acetate in step 5) are as follows: the mass volume ratio of the oleuropein crude product to the ethyl acetate is 1 g: 8-10mL, and the hot melting temperature is 45-50 ℃.
9. The method according to claim 1, wherein the low-temperature standing condition in the step 5) is: the low temperature is 0-5 ℃, and the standing time is 12-24 hours.
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| CN109125182A (en) * | 2018-10-16 | 2019-01-04 | 阿谷巴科技（唐山）有限公司 | A kind of Cleupin cold cream and preparation method thereof with bacteriostasis |
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| CN102702287A (en) * | 2012-06-21 | 2012-10-03 | 桂林三宝药业有限公司 | Method for extracting purified oleuropein from olive leaves |
| CN102850416A (en) * | 2012-09-07 | 2013-01-02 | 中国林业科学研究院林产化学工业研究所 | Method and apparatus used for preparing olive leaf extract |
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| CN102702287A (en) * | 2012-06-21 | 2012-10-03 | 桂林三宝药业有限公司 | Method for extracting purified oleuropein from olive leaves |
| CN102850416A (en) * | 2012-09-07 | 2013-01-02 | 中国林业科学研究院林产化学工业研究所 | Method and apparatus used for preparing olive leaf extract |
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| Title |
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| 橄榄苦苷提取工艺的研究进展;谢普军等;《生物质化学工程》;20120531;第46卷(第3期);第33-37页 * |
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