CN105753927A - Method for extracting oleanolic acid from talinum crassifolium - Google Patents
Method for extracting oleanolic acid from talinum crassifolium Download PDFInfo
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- CN105753927A CN105753927A CN201610194539.4A CN201610194539A CN105753927A CN 105753927 A CN105753927 A CN 105753927A CN 201610194539 A CN201610194539 A CN 201610194539A CN 105753927 A CN105753927 A CN 105753927A
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- oleanolic acid
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- ethanol
- talini paniculati
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- MIJYXULNPSFWEK-GTOFXWBISA-N 3beta-hydroxyolean-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MIJYXULNPSFWEK-GTOFXWBISA-N 0.000 title claims abstract description 57
- JKLISIRFYWXLQG-UHFFFAOYSA-N Epioleonolsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4CCC3C21C JKLISIRFYWXLQG-UHFFFAOYSA-N 0.000 title claims abstract description 57
- YBRJHZPWOMJYKQ-UHFFFAOYSA-N Oleanolic acid Natural products CC1(C)CC2C3=CCC4C5(C)CCC(O)C(C)(C)C5CCC4(C)C3(C)CCC2(C1)C(=O)O YBRJHZPWOMJYKQ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- MIJYXULNPSFWEK-UHFFFAOYSA-N Oleanolinsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MIJYXULNPSFWEK-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229940100243 oleanolic acid Drugs 0.000 title claims abstract description 57
- HZLWUYJLOIAQFC-UHFFFAOYSA-N prosapogenin PS-A Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC1OCC(O)C(O)C1O HZLWUYJLOIAQFC-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 33
- 235000015055 Talinum crassifolium Nutrition 0.000 title abstract 4
- 244000099346 Talinum fruticosum Species 0.000 title abstract 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003208 petroleum Substances 0.000 claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 18
- 239000000284 extract Substances 0.000 claims description 17
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
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- WCGUUGGRBIKTOS-GPOJBZKASA-N (3beta)-3-hydroxyurs-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C WCGUUGGRBIKTOS-GPOJBZKASA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- 108010059892 Cellulase Proteins 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- PLSAJKYPRJGMHO-UHFFFAOYSA-N ursolic acid Natural products CC1CCC2(CCC3(C)C(C=CC4C5(C)CCC(O)C(C)(C)C5CCC34C)C2C1C)C(=O)O PLSAJKYPRJGMHO-UHFFFAOYSA-N 0.000 description 2
- 229940096998 ursolic acid Drugs 0.000 description 2
- UUTKICFRNVKFRG-WDSKDSINSA-N (4R)-3-[oxo-[(2S)-5-oxo-2-pyrrolidinyl]methyl]-4-thiazolidinecarboxylic acid Chemical compound OC(=O)[C@@H]1CSCN1C(=O)[C@H]1NC(=O)CC1 UUTKICFRNVKFRG-WDSKDSINSA-N 0.000 description 1
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- 101710098398 Probable alanine aminotransferase, mitochondrial Proteins 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 244000297179 Syringa vulgaris Species 0.000 description 1
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- VBICKXHEKHSIBG-UHFFFAOYSA-N beta-monoglyceryl stearate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a method for extracting oleanolic acid from talinum crassifolium.After fatting, alcohol extraction and decompressing concentration are conducted on petroleum ether, ethyl acetate is extracted, and then a column chromatography method and a crystallization method are adopted to obtain an oleanolic acid product high in purity.By means of the method, the oleanolic acid in roots and stems of the talinum crassifolium can be fully utilized, the production cost of the oleanolic acid is effectively lowered, and main active ingredients in the roots and stems of the talinum crassifolium are fully utilized.Column chromatography and crystallization are combined, excessive consumption of chemical reagent is reduced, the pure natural property of a product is guaranteed, and the oleanolic acid can be safely provided for industries such as food, cosmetics and pharmacy.
Description
Technical field
The invention belongs to technical field of natural product extraction, a kind of method relating to extracting oleanolic acid in the Radix Talini Paniculati's of employing root and stem.
Background technology
Radix Talini Paniculati, has another name called: smoke tree orchid, Silene tatarinowii Regel-Melandrium tatarinwiii (Regel) Tsui., Radix angelicae morii, the period of the day from 3 p.m. to 5 p.m. flower, flower of cooking, Panax pseudoginseng Wall., ginseng Korean Ginseng careless, native, water Radix Ginseng, purple Radix Ginseng etc., belong to Centrospermae, Portulacaceae is annual or perennial herb.Strain is without hair, high 30-100 centimetre.Main root is sturdy, cone, has minority branch, skin pitchy, section milky.Stem is upright, meat, and base portion is closely wooden, how many branches, cylindrical, sometimes has groove.Leaf alternate or near blade is meat slightly to life, tool short handle or nearly stockless, obovate or the shape of falling ovum oblong, long 5-10 centimetre, wide 2.5-5 centimetre, the anxious point in top, nick sometimes, tool mucro, the narrow wedge shape of base portion, Quan Yuan.Panicle top is raw or axil is raw, bigger shape, and normal two dichotomies have long peduncle；Spend little, diameter about 6 millimeters；Phyllary is green or closely red, and circular, nose-circle is blunt, long 3-4 millimeter；Bract 2, film quality, lanceolar, the anxious point in top, it is about 1 millimeter；The long 5-10 millimeter of bennet；Sepal is avette, aubergine, caducous；Petal pink or lilac red, oblong, obovate or ellipse, long 6-12 millimeter, nose-circle is blunt, rare nick；Stamen (10-) 15-20 is shorter than petal；Style is linear, is about 2 millimeters, base portion tool joint；Stigma 3 splits, and slightly carries out；Ovary ovoid, is about 2 millimeters.Capsule is subsphaeroidal, diameter about 4 millimeters, and 3 lobes split, hard papery；Seed majority, oblateness, diameter about 1 millimeter, pitchy or black are glossy.The month at florescence 6-7, fruit month phase 9-10.Root is used as medicine, strengthening by means of tonics.Radix Talini Paniculati cultivates easily, and rapidly, sick few worm is micro-in breeding, and the equal edible of root, leaf can be fried, can cook soup, can rinse, can stew, medicine vegetables dual-purpose.It is hotel vegetable as the young stem and leaf that the edible part of vegetable is constantly growth.Fleshy tap root, is a kind of medicinal tonic, has strengthening by means of tonics effect, spleen invigorating lung moistening, cough-relieving, regulating menstruation.For insufficiency of the spleen overstrain, have loose bowels, impairment of the lung caused by overstrain cough with blood-flecked phlegm, dizziness hectic fever, night sweat spontaneous perspiration, menoxenia, leukorrhagia.Invigorating the spleen and replenishing QI, the lung moistening and production of body fluid promoting.Weak for the deficiency of vital energy, body void spontaneous perspiration, diarrhea due to hypofunction of the spleen, xeropulmonary cough, milk is rare.Containing effective active components such as oleanolic acid, stearic acid monoglyceride, cupreols in Radix Talini Paniculati's rhizome.
Oleanolic acid is used for treating infectious acute icterohepatitis, has and significantly reduces glutamate pyruvate transaminase and jaundice eliminating effect, improves viral and chronic persistent hepatitis patient symptom, sign and liver function；Can be additionally used in psoriasis, rheumatic arthritis, oedema due to nephritis, cirrhotic ascites, acute, chronic hepatitis, stranguria with turbid discharge of having a stomachache, metrorrhagia, traumatic injury, carbuncle, soreness of the waist and knees, the disease such as frequent fetal movement.
Publication number is that CN1045585 Chinese patent discloses a kind of method extracting oleanolic acid from plant, it is characterised in that it is completed by following steps: a, and water carries, and the plant containing the triterpenoid saponin being oleanolic acid adds water, with smothered with, then concentrated aqueous solution；B, hydrolysis: the aqueous solution to concentration adds concentrated sulphuric acid, adds pyrohydrolysis.C, acid alcohol liquid recrystallization；Water-insoluble ethanol or methanol dissolve, and filter, adjust PH10～11 with NaOH, go precipitation, take supernatant, add Hcl to alcoholic solution 1/2～1/5 or add 1/5～the dense H of the water of 1/2 alcoholic solution volume and 1/10～1/15 alcoholic solution volume2SO4, reflux, stand crystallization, filter, take screening and be and teach fruit acid together.
Publication number is that CN101450962 Chinese patent discloses a kind of method extracting oleanolic acid from Kandelia candel leaf, comprises the steps: to dry in the shade after Kandelia candel leaf cleaning, adds dichloromethane extraction, filter to obtain extracting solution, dry, obtains extractum；Extractum is added silica gel for chromatography absorption, grinds into powder, fill post, with petroleum ether/acetone for eluant, carry out gradient elution, in mass ratio, with petroleum ether: acetone respectively 30: 1,10: 1 and 4: 1, rush 1～5 column volume, finally with washed with methanol, there are 18 components, the 12nd～17 component therein is oleanolic acid crude product, then through silica gel column chromatography, carry out eluting with chloroform/methanol for eluant, finally with washed with methanol, there are 4 components, the 3rd component therein is oleanolic acid sterling.
Publication number is that CN101857625A Chinese patent discloses a kind of method extracting oleanolic acid from Fructus Hippophae, comprises the steps: the pre-treatment of (1) sea buckthorn fruit；(2) extraction of ursolic acid and oleanolic acid；(3) separation of fruit acid and oleanolic acid.A kind of method extracting oleanolic acid from Fructus Hippophae of the present invention has the advantages that compared with prior art: the present invention utilizes supercritical carbon dioxide fluid extraction to extract ursolic acid and oleanolic acid from seabuckthorn fruit peel, reach most optimum distribution of resources, improve the purpose of Fructus Hippophae series products added value.
Publication number is that CN103059092A Chinese patent discloses a kind of method extracting oleanolic acid from Fructus Chaenomelis, and after (1) takes the drying of the Fructus Chaenomelis slag after squeezing the juice, the ratio of 1:2 is squeezed after putting into and soaking 2 hours in warm water in mass ratio；Filter cake slag after drying more in mass ratio the ratio of 1:2 put in warm water soak, it is separately added into the compound enzyme of pectase, cellulase and hemicellulase simultaneously, mass ratio is 1:2:3, and addition is 1000u/100g filter cake slag, and enzymolysis is filter cake slag dry for standby after 3 hours；(2) ratio of dry Fructus Chaenomelis filter cake slag 1:3 in mass ratio being put into decompression in the ethanol of 95%vol extract 2 hours, repeat respectively to extract 2 times, extract vacuum concentrates, and obtains paste；(3) paste is added pure water, carry out alkali extraction and acid precipitation, spray drying, recrystallization, obtain oleanolic acid sterling.Present invention process is simpler, and oleanolic acid extraction ratio and purity are higher.
nullPublication number is that CN103483412A Chinese patent discloses a kind of new method extracting oleanolic acid from Fructus Ligustri Lucidi，It is specifically related to a kind of method that enzymolysis combines with condensation technique，The alcoholic solution of the 70～90% of addition 10～15 times in the Fructus Ligustri Lucidi pulverized，Adding hydrochloric acid adjusts pH value to be 3～5，Continuously add the cellulase degradation of 0.03～0.05%，Adding alkali adjusts pH value for neutrality，Put into hermetic container，10～15min is extracted when pressure is 20～30MPa，Extracting solution filters，Filter after adding activated carbon decolorizing，Filtrate concentration is the 1/10～15 of former solvent volume，The macroporous adsorbent resin of pretreatment on concentrated solution，With the ethanol elution of 90～100%，Eluent concentrating under reduced pressure obtains crude product，Recrystallizing methanol obtains acicular crystal oleanolic acid.Reaction condition of the present invention is gentle, extraction ratio is high, extraction time is short, extraction cost is low, it is adaptable to industrialized production.
Publication number is that CN104478985A Chinese patent discloses a kind of method extracting oleanolic acid from Japan's wood blade, step is as follows: is added in extracting solution by Japan's wood blade particle and is heated to 90-95 DEG C, until mixeding liquid volume reduces to 1/5th, liquid after separation and Extraction, then rejoin extracting solution and be heated to 90-95 DEG C in Japan's wood blade powder, until mixeding liquid volume reduces to 1/5th, repeat said extracted process 3-4 time；Liquid after united extraction, is cooled to room temperature, obtains filtrate through membrane filtration；Filtrate being mixed with deionized water, 90 DEG C of water-baths make ethanol volatilize until there is light brown serosity；Being extracted by serosity ether, then 70 DEG C of water-baths are until ether volatilization completely, obtains oleanolic acid extract.The present invention advantage be: should extracting the method technique of oleanolic acid efficiency short, that extract simple, consuming time from Japan's wood blade high, testing result shows: through extracting for 3 times, 2 hours used times, and extraction ratio can reach 99.81%.
Publication number is that CN104592343A Chinese patent discloses a kind of method extracting oleanolic acid from Spica Prunellae, comprises the following steps: pulverized by dry Spica Prunellae, adds alcohol reflux, and concentrating under reduced pressure obtains extractum A；Add petroleum ether drip washing, ethanol dissolution filter, be easily separated through simulated moving bed chromatography, obtain the component B rich in oleanolic acid；The oleanolic acid of dry purity more than 95%.Oleanolic acid extracting method of the present invention, adopts the technique that microwave radiation exaraction and simulated moving bed chromatography method separating-purifying combine, it is determined that related process parameters, and step is simple, and product purity is higher, extracts disengaging time shorter, and production efficiency is improved.
At present, have from the plants such as Fructus Crataegi, Fructus Chaenomelis, Spica Prunellae and Fructus Ligustri Lucidi, extract highly purified oleanolic acid, but extract, Radix Talini Paniculati, the method separating oleanolic acid and have no documents and materials report.
Summary of the invention
The present invention provides a kind of method extracting oleanolic acid from Radix Talini Paniculati's rhizome, comprises the steps:
(1) after pulverizing, Radix Talini Paniculati's rhizome carries out room temperature lixiviate with the petroleum ether of twice to four times of weight, filters and removes petroleum ether lixiviating solution, obtains Radix Talini Paniculati's residue.
(2) Radix Talini Paniculati's residue addition ethanol carries out 50～70 DEG C of reflux, extract, 1～4h, and filter cleaner obtains filtrate I, takes filtrate I and carries out vacuum at 50 DEG C～65 DEG C or be evaporated to the 1/10～1/25 of original volume, it is thus achieved that concentrated solution I.
(3) being extracted by ethyl acetate by concentrated solution I, be extracted liquid I, wherein the volume L of concentrated solution I is 1:1～4 with the volume L ratio of ethyl acetate.
(4) LSA-20 macroporous resin column on extract I is adsorbed, carry out post eluting with the ethanol water of three times to five times column volumes, obtain eluent I.
(5) eluent I carrying out vacuum at 50 DEG C～65 DEG C or is evaporated to the 1/5～1/15 of original volume, room temperature stands 15～50min, filters, obtains filtering residue and be oleanolic acid crude product.
(6) adding acetone to oleanolic acid crude product and heat 10～20min, while hot ceramic membrane filter at 40 DEG C, filtrate places refrigerator overnight, and crystallization, recrystallization once, obtains oleanolic acid.
In one embodiment, described filtration is filtered through gauze, ceramic membrane filter, wherein, it will be preferred that three layers filtered through gauze 2 times, ceramic membrane filter 1 time.
In a specific embodiment, ethanol described in step (2) makes consumption, and by volume/Radix Talini Paniculati's rhizome weight ratio is 2～6L:1kg.
In a specific embodiment, ethanol water described in step (4) is the aqueous solution containing 70～90% ethanol；The water that compound method such as 70% ethanol water is 70mL dehydrated alcohol addition 30mL mixes.
In a specific embodiment, acetone volume described in step (6) and oleanolic acid crude product weight ratio are 1～3L:1kg.
Above-mentioned LSA-20 macroporous resin used is bought from Zhengzhou Qin Shi Science and Technology Ltd..
Technique effect
1, the present invention can make oleanolic acid in Radix Talini Paniculati's rhizome be fully used, and effectively reduces its production cost, takes full advantage of main active ingredient in Radix Talini Paniculati's rhizome.
2, be combined with crystalline phase by column chromatography, reduce the excessive use of chemical reagent, it is ensured that the pure natural property of product, it is possible to safe is supplied to the industries such as food, cosmetics and pharmacy.
Detailed description of the invention
Below, the present invention will be further detailed by embodiment, but it is not limited to any one or similar example of these embodiments.
Embodiment 1:
After pulverizing, Radix Talini Paniculati's rhizome 100kg and petroleum ether 300kg carries out room temperature lixiviate, filters and removes petroleum ether lixiviating solution, obtains Radix Talini Paniculati's residue.Radix Talini Paniculati's residue adds 400L ethanol and carries out 50～70 DEG C of reflux, extract, 2h, and filter cleaner obtains 350L filtrate I, takes filtrate I and carries out vacuum or concentrating under reduced pressure at 60 DEG C, it is thus achieved that 20L concentrated solution I.Concentrated solution I 40L ethyl acetate is extracted, is extracted liquid I.LSA-20 macroporous resin column on extract I is adsorbed, carries out post eluting with 85% ethanol water of three times to five times column volumes, obtain 140L eluent I.Eluent I carrying out vacuum at 60 DEG C or is evaporated to 15L, room temperature stands 40min, filters, obtains filtering residue and be oleanolic acid crude product 1.84kg.Adding 3L acetone to oleanolic acid crude product and heat 15min, while hot ceramic membrane filter at 40 DEG C, filtrate places refrigerator overnight, crystallization, and recrystallization once, obtains oleanolic acid 1.46kg, detects through HPLC, and the purity of oleanolic acid sample is 97.25%.
Embodiment 2
After pulverizing, Radix Talini Paniculati's rhizome 200kg and petroleum ether 500kg carries out room temperature lixiviate, filters and removes petroleum ether lixiviating solution, obtains Radix Talini Paniculati's residue.Radix Talini Paniculati's residue adds 700L ethanol and carries out 50～70 DEG C of reflux, extract, 1～4h, and filter cleaner obtains 660L filtrate I, takes filtrate I and carries out vacuum or concentrating under reduced pressure at 55 DEG C, it is thus achieved that 35L concentrated solution I.Concentrated solution I 50L ethyl acetate is extracted, is extracted liquid I.LSA-20 macroporous resin column on extract I is adsorbed, carries out post eluting with 80% ethanol water of three times to five times column volumes, obtain 180L eluent I.Eluent I carrying out vacuum at 55 DEG C or is evaporated to 20L, room temperature stands 50min, filters, obtains filtering residue and be oleanolic acid crude product 3.98kg.Adding 6L acetone to oleanolic acid crude product and heat 20min, while hot ceramic membrane filter at 40 DEG C, filtrate places refrigerator overnight, crystallization, and recrystallization once, obtains oleanolic acid 2.94kg, detects through HPLC, and the purity of oleanolic acid sample is 97.46%.
Embodiment 3
After pulverizing, Radix Talini Paniculati's rhizome 400kg and petroleum ether 1000kg carries out room temperature lixiviate, filters and removes petroleum ether lixiviating solution, obtains Radix Talini Paniculati's residue.Radix Talini Paniculati's residue adds 1000L ethanol and carries out 50～70 DEG C of reflux, extract, 3h, and filter cleaner obtains 900L filtrate I, takes filtrate I and carries out vacuum or concentrating under reduced pressure at 60 DEG C, it is thus achieved that 50L concentrated solution I.Concentrated solution I 80L ethyl acetate is extracted, is extracted liquid I.LSA-20 macroporous resin column on extract I is adsorbed, carries out post eluting with 85% ethanol water of three times to five times column volumes, obtain 250L eluent I.Eluent I carrying out vacuum at 55 DEG C or is evaporated to 20L, room temperature stands 40min, filters, obtains filtering residue and be oleanolic acid crude product 8.45kg.Adding 15L acetone to oleanolic acid crude product and heat 15min, while hot ceramic membrane filter at 40 DEG C, filtrate places refrigerator overnight, crystallization, and recrystallization once, obtains oleanolic acid 6.28kg, detects through HPLC, and the purity of oleanolic acid sample is 97.58%.
Claims (5)
1. the present invention provides a kind of method extracting oleanolic acid from Radix Talini Paniculati's rhizome, comprises the steps:
(1) after pulverizing, Radix Talini Paniculati's rhizome carries out room temperature lixiviate with the petroleum ether of twice to four times of weight, filters and removes petroleum ether lixiviating solution, obtains Radix Talini Paniculati's residue.
(2) Radix Talini Paniculati's residue addition ethanol carries out 50～70 DEG C of reflux, extract, 1～4h, and filter cleaner obtains filtrate I, takes filtrate I and carries out vacuum at 50 DEG C～65 DEG C or be evaporated to the 1/10～1/25 of original volume, it is thus achieved that concentrated solution I.
(3) being extracted by ethyl acetate by concentrated solution I, be extracted liquid I, wherein the volume L of concentrated solution I is 1:1～4 with the volume L ratio of ethyl acetate.
(4) LSA-20 macroporous resin column on extract I is adsorbed, carry out post eluting with the ethanol water of three times to five times column volumes, obtain eluent I.
(5) eluent I carrying out vacuum at 50 DEG C～65 DEG C or is evaporated to the 1/5～1/15 of original volume, room temperature stands 15～50min, filters, obtains filtering residue and be oleanolic acid crude product.
(6) adding acetone to oleanolic acid crude product and heat 10～20min, while hot ceramic membrane filter at 40 DEG C, filtrate places refrigerator overnight, and crystallization, recrystallization once, obtains oleanolic acid.
2. method according to claim 1, described filtration is filtered through gauze, ceramic membrane filter, wherein, it will be preferred that three layers filtered through gauze 2 times, ceramic membrane filter 1 time.
3. method according to claim 1, ethanol described in step (2) makes consumption, and by volume/Radix Talini Paniculati's rhizome weight ratio is 2～6L:1kg.
4. method according to claim 1, ethanol water described in step (4) is the aqueous solution containing 70～90% ethanol.
5. method according to claim 1, acetone volume described in step (6) and oleanolic acid crude product weight ratio are 1～3L:1kg.
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Correction item: Patentee|Address|Patentee Correct: Jishou University|416000 No. 120 Renmin South Road, Jishou City, Hunan Province|Tongren University False: Jishou University|541001 93 Xinyi Road, Xiufeng District, Guilin, the Guangxi Zhuang Autonomous Region|Tongren University Number: 51-01 Volume: 33 |
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