CN104031113A - Method for preparing high-purity oleanolic acid from Aralia taibaiensis - Google Patents
Method for preparing high-purity oleanolic acid from Aralia taibaiensis Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity oleanolic acid from Aralia taibaiensis, belonging to the technical field of natural product extraction separation. The method comprises the following steps: 1) washing an Aralia taibaiensis oleanolic acid crude product with water, taking the insoluble substance, adding analytic methanol into the insoluble substance, sufficiently and evenly mixing, filtering, and taking the supernatant to obtain a loading solution; 2) filling a high-pressure preparative liquid chromatography column with octadecylsilane bonded silica gel, loading the loading solution to the high-pressure preparative liquid chromatography column, and eluting by using a methanol-water system as an eluate; and 3) carrying out sectional collection under the detection of an ultraviolet detector to obtain an oleanolic acid solution, concentrating the oleanolic acid solution under reduced pressure, and washing with water to obtain the high-purity oleanolic acid. The method can be used for directly and quickly separating out the oleanolic acid, and has the advantages of short separation time and high separation quantity; the yield is up to 85% above, and the purity is up to 98% above; and the method has the characteristics of less generated waste, small required eluate volume, recyclable filler and solvent and environment friendliness, and is suitable for industrial production.
Description
Technical field
The invention belongs to natural product extraction separation technology field, be specifically related to a kind of from Tai Bai Aralia wood the method for separation and Extraction Oleanolic Acid.
Background technology
Too white Aralia wood has another name called Caulis et Folium Pothi Repentis, is five to add section's Aralia wood and belong to perennial plant, is distributed in the west area of China, has very abundant wild resource.The white skin of Tai Bai Aralia wood Yi Cheng Aralia wood, the white skin of Chinese medicine voluminous dictionary Yi Aralia wood records.This medicinal material has stomach invigorating convergence diuresis and sugaring effect, can mend waist kidney, the multiple efficacies such as Ji invigorates blood circulation strengthen the bone, relax.
Oleanolic Acid, the clinical infectivity acute icterohepatitis that is used for the treatment of, has obvious reduction gpt and removing jaundice effect, improves viral and symptom chronic persistent hepatitis patient, sign and liver function; Also can be used for psoriatic, rheumatic arthritis, nephritic edema, hepatic ascites, acute, chronic hepatitis, stomachache stranguria with turbid discharge, metrorrhagia, wound, carbuncle is swollen, soreness of the waist and knees, the diseases such as threatened abortion.
At present, the extracting method that Oleanolic Acid has been reported aspect separation and purification mainly taking organic solution lixiviate in conjunction with certain separation means as main, but can only obtain Oleanolic Acid crude product.Preparation cycle is long and cost is higher, based on above reason development of new separation purifying technique, find more economically, efficiently, separating and purifying technology efficiently, more and more become the focus that investigator pays close attention to.
Summary of the invention
The object of the present invention is to provide a kind of from Tai Bai Aralia wood the method for separating high-purity Oleanolic Acid, the method is simple to operate, disengaging time is short, cost is low, the product purity obtaining is high, yield is high.
The present invention is achieved through the following technical solutions:
A method of preparing high purity oleanolic acid from Tai Bai Aralia wood, comprises the following steps:
1) washing of will be too white Aralia wood Oleanolic Acid crude product, gets insolubles, according to 1g:(3～7) solid-liquid ratio of mL, in insolubles, add analysis methyl alcohol, fully mix, cross leaching supernatant, obtain sample solution;
2) fill after high pressure preparative liquid chromatography post with octadecylsilane chemically bonded silica, sample solution is splined on to high pressure preparative liquid chromatography post, taking methanol-water system as elutriant, with speed isorheic elution 30～40min of 10～200mL/min; In described elutriant, the volume ratio of methyl alcohol and water is (90～97): (10～3);
3) under detecting, UV-detector carries out Fractional Collections according to chromatogram appearance time, in the time that starting to rise, collects at the corresponding peak of Oleanolic Acid, when dropping to, this peak finishes five of whole peak height/a period of time to collect, obtain olea acid solution, olea acid solution is evaporated to without methyl alcohol taste, precipitate is washed with boiling water, obtains high purity oleanolic acid.
Step 2) described loading employing gradation loading, each loading 10～20mL.
The particle diameter of described octadecylsilane chemically bonded silica is 5～20 μ m; Column length 15～the 25cm of high pressure preparative liquid chromatography post; It is 210nm that described high pressure liquid chromatography post detects wavelength.
Step 3) described olea acid solution concentrating under reduced pressure is at 40～60 DEG C, under the condition that vacuum tightness is 0.09～0.15Mpa, carries out.
The preparation of described Tai Bai Aralia wood Oleanolic Acid crude product comprises the following steps:
1) by pretreated too white Aralia wood medicinal material with filtering after water extraction, get filter residue, after the ethanolic soln refluxing extraction that is 85%～95% with massfraction by filter residue, filtration again, obtains ethanol extract;
2) by ethanol extract activated carbon decolorizing, then filtering gac, then regulate ethanol extract pH value to alkalescence, and filtering and impurity removing after leaving standstill, filters after filtrate decompression is concentrated again, and get is Dao Aralia wood Oleanolic Acid crude product.
Described pretreated Tai Bai Aralia wood medicinal material is that the stem skin of Tai Bai Aralia wood and root are obtained after washing, dry and pulverization process.
Step 1) described with water extraction be by pretreated too white Aralia wood medicinal material flooding three times, each 1～2h, wherein, the amount ratio of the wooden medicinal material of pretreated too white Aralia and water is 1g:(10～15) mL; The number of times of described refluxing extraction is 2～3 times, each 1.5～2h, wherein, the amount ratio of the ethanolic soln that pretreated Tai Bai Aralia wood medicinal material and massfraction are 85%～95% is 1g:(8～12) mL.
Step 2) be to regulate ethanol extract pH value to 9～11 with 0.5～1.0mol/L aqueous sodium hydroxide solution.
Step 2) in the volume of filtrate decompression after concentrated be 1/3～1/5 of concentrated front volume; Concentrating under reduced pressure is at 40～60 DEG C, under the condition that vacuum tightness is 0.09～0.15Mpa, carries out.
Step 2) consumption of active carbon for decolorization is 0.1%～1.0% of ethanol extract volume, decolouring is at 50～70 DEG C, fully stirs 15～60min; Repeat to add activated carbon decolorizing to process 2～3 times.
Compared with prior art, the present invention has following useful technique effect:
The present invention separates first Application in the extraction process of Tai Bai Aralia wood Oleanolic Acid by high pressure preparative chromatography, use octadecylsilane chemically bonded silica is high pressure preparative chromatography column packing, success separates and obtains high purity oleanolic acid, in sepn process, only use this kind of chromatogram system of first alcohol and water, carry out constant current constant speed Gradient elution, adopt UV-detector on-line monitoring method separated product and impurity, can accomplish accurate collection, the inventive method sepn process simple and fast, flash liberation just can achieve the goal, without any need for chemical treatment method, can not lose Oleanolic Acid, can be directly, separate and obtain Oleanolic Acid fast, and disengaging time is short, fractional dose is large, and the Oleanolic Acid purity obtaining is up to more than 98%.
The waste material that the inventive method produces is few, and post effect is high, and required effluent volume is little, and floor space is little, has reduced the consuming cost of whole technique, solvent recoverable, and environmental friendliness, is applicable to suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the Fractional Collections Oleanolic Acid of the present invention HPLC color atlas of each composition in product roughly;
Fig. 2 is the HPLC mensuration chromatic graph spectrum that the present invention separates the Oleanolic Acid obtaining.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
The reagent that the present invention is used and laboratory apparatus
1, reagent: preparation is analytical pure with sodium hydroxide, ethanol, methyl alcohol, hydrochloric acid, analysis is chromatographically pure with acetonitrile, water is secondary redistilled water;
2, laboratory apparatus: it is U.S.'s Agilent high-pressure chromatographic column that the present invention has adopted major diameter preparative column, it is Agilent company product that high pressure is prepared liquid phase systems, preparation is Agilent product by UV-detector, automatically fraction collection system is that Agilent is produced, and product analysis is used high performance liquid chromatograph for the U.S. (Waters) production.
Technical scheme of the present invention is as follows:
A method for separating high-purity Oleanolic Acid from Tai Bai Aralia wood, comprises the following steps:
1) washes Aralia wood stem skin and root totally with water, dries, then pulverize, again taking pure water as extracting solution lixiviate three times, filter, remove the water-soluble impurity such as carbohydrate, tannin, the dregs of a decoction, so that the ethanolic soln as 85%～95% filters after solvent refluxing extracts with massfraction, are obtained to ethanol extract;
2) by ethanol extract activated carbon decolorizing, filtering gac, regulating ethanol extract pH value with 1.0mol/L aqueous sodium hydroxide solution is 11 left and right, leave standstill after impurity screening, at 40～60 DEG C, vacuum tightness reaches 0.09～0.15Mpa and concentrates filtrate to the small volume 1/3-1/5 of front volume (concentrated), filters, and leaches Wu Wei Aralia wood Oleanolic Acid crude product;
3) Tai Bai Aralia wood Oleanolic Acid crude product is washed with pure water, is got insolubles, by insolubles with analyze methyl alcohol according to 1g:(5～10) solid-liquid ratio of mL, after fully mixing, filter, remove insolubles, obtain sample solution;
4) sample solution gradation is splined on to high pressure and prepares liquid phase and separate, chromatographic column is taking octadecylsilane chemically bonded silica as weighting agent, taking methanol-water system as elutriant; Detection wavelength is 210nm; With speed isorheic elution 30～40min of 10～200ml/min, in described elutriant, the volume ratio of methyl alcohol and water is (90～97): (10～3); Described gradation loading is each loading 10～20ml sample;
5) under detecting, UV-detector carries out Fractional Collections according to chromatogram appearance time, in the time that starting to rise, collects at the corresponding peak of Oleanolic Acid, when dropping to, this peak finishes five of whole peak height/a period of time to collect, obtain olea acid solution, at 40-60 DEG C, vacuum tightness reaches 0.09～0.15Mpa, and olea acid solution is evaporated to without methyl alcohol taste, and precipitate can obtain highly purified Oleanolic Acid with the distilled water washing of boiling;
In chromatographic separation of the present invention, Oleanolic Acid peak type is more symmetrical, but peak do not reach when therefore baseline separation starts to rise at peak in sepn process and collect, peak drop to whole high by five/finish for the moment to collect.
The Oleanolic Acid elutriant of collecting in chromatographic separation process, by Rotary Evaporators at 40～60 DEG C, vacuum tightness is under 0.09～0.15Mpa, reclaim solvent, precipitate can obtain highly purified Oleanolic Acid with the distilled water washing of boiling, by high performance liquid chromatography quantitative analysis purity more than 98%.
Through chromatographic separation repeatedly, the separator column effect of high pressure preparative liquid chromatography post reduces, the hydrochloric acid soln that now available quality concentration is 5% carries out counterflush preparative column, column flow rate is 10～20% of chromatographic separation flow velocity, then use 3% acetonitrile solution to wash away chlorion unnecessary in chromatographic column, recover chromatographic column post effect.
Embodiment 1
A method for separating high-purity Oleanolic Acid from Tai Bai Aralia wood, comprises the following steps:
1) get Tai Bai Aralia wood rhizome dry product 1Kg, wash with water totally, dry, pulverize; Join 10L water boil 1.5 hours, the water cooking liquid that inclines, the dregs of a decoction divide refluxing extraction 3 times with 95% ethanol, and each ethanol consumption is 6L;
2) merge the gac that alcohol extract adds alcohol extract volume 0.3%, at 50 DEG C, stir decolouring 1 hour; Filtering gac, it is 11 left and right that decolouring alcohol extract regulates ethanol extract pH value with 1.0mol/L aqueous sodium hydroxide solution, leave standstill after 12 hours and filter, except precipitation, after impurity screening, filtrate is at 40 DEG C, vacuum tightness reaches 0.15Mpa and concentrates filtrate to 1/3 left and right (5L) that concentrates front volume, have a large amount of insolubless to separate out, filter, leaching insolubles is Oleanolic Acid crude product 8.6g;
3) Oleanolic Acid crude product 8.6g obtained above is washed with appropriate pure water, water-insoluble is analyzed dissolve with methanol with 50ml, after fully mixing, filters, and removes insolubles, obtains sample solution;
4) sample solution gradation is splined on to high pressure and prepares liquid phase and separate, chromatographic column is taking octadecylsilane chemically bonded silica as weighting agent, taking methanol-water system as elutriant; Detection wavelength is 210nm; With speed isorheic elution 30～40min of 20ml/min, in described elutriant, the volume ratio of methyl alcohol and water is 97:3; Described gradation loading is each loading 10～20ml sample;
5) under detecting, UV-detector carries out Fractional Collections according to chromatogram appearance time, observe chromatographic peak by software, in the time that starting to rise, collects at the corresponding peak of Oleanolic Acid, on 8.4min Oleanolic Acid product peak, rise, collect by automatic fraction collector, referring to Fig. 1, collection time is that Oleanolic Acid peak starts ascent stage 8.45 minutes, and the peak whole peak height 1/5th that declines finishes to collect.After 30min, finish this elution system, carry out the collection of repetition sample introduction, until the Oleanolic Acid sample solution sample introduction of preparation is complete, collect liquid and in Rotary Evaporators, reclaim solvent, at 40 DEG C, vacuum tightness reaches 0.15Mpa, and olea acid solution is evaporated to without methyl alcohol taste, and precipitate can obtain highly purified Oleanolic Acid with the distilled water washing of boiling; Obtain dried powder 1.03g, by high performance liquid chromatography quantitative analysis, referring to Fig. 2, content of oleanolic acid is 98.9%.
Embodiment 2
A method for separating high-purity Oleanolic Acid from Tai Bai Aralia wood, comprises the following steps:
1) get Tai Bai Aralia wood rhizome dry product 1Kg, wash with water totally, dry, pulverize; Join 12L water boil 1.0 hours, the water cooking liquid that inclines, the dregs of a decoction divide refluxing extraction 3 times with 90% ethanol, and each ethanol consumption is 8L;
2) merge the gac that alcohol extract adds alcohol extract volume 0.6%, at 60 DEG C, stir decolouring 0.8 hour; Filtering gac, it is 11 left and right that decolouring alcohol extract regulates ethanol extract pH value with 0.6mol/L aqueous sodium hydroxide solution, leave standstill after 10 hours and filter, except precipitation, after impurity screening, filtrate is at 55 DEG C, vacuum tightness reaches 0.12Mpa and concentrates filtrate to 1/4 left and right (6L) that concentrates front volume, have a large amount of insolubless to separate out, filter, leaching insolubles is Oleanolic Acid crude product 8.1g;
3) Oleanolic Acid crude product 8.1g obtained above is washed with appropriate pure water, water-insoluble is analyzed dissolve with methanol with 70ml, after fully mixing, filters, and removes insolubles, obtains sample solution;
4) sample solution gradation is splined on to high pressure and prepares liquid phase and separate, chromatographic column is taking octadecylsilane chemically bonded silica as weighting agent, taking methanol-water system as elutriant; Detection wavelength is 210nm; With the speed isorheic elution 40min of 40ml/min, in described elutriant, the volume ratio of methyl alcohol and water is 95:5; Described gradation loading is each loading 10～20ml sample;
5) under detecting, UV-detector carries out Fractional Collections according to chromatogram appearance time, observe chromatographic peak by software, in the time that starting to rise, collects at the corresponding peak of Oleanolic Acid, on 8.7min Oleanolic Acid product peak, rise, collect by automatic fraction collector, collection time is that Oleanolic Acid peak starts ascent stage 8.75 minutes, and the peak whole peak height 1/5th that declines finishes to collect.After 40min, finish this elution system, carry out the collection of repetition sample introduction, until the Oleanolic Acid sample solution sample introduction of preparation is complete, collect liquid and in Rotary Evaporators, reclaim solvent, at 50 DEG C, vacuum tightness reaches 0.10Mpa, and olea acid solution is evaporated to without methyl alcohol taste, and precipitate can obtain highly purified Oleanolic Acid with the distilled water washing of boiling; Obtain dried powder 0.96g, by high performance liquid chromatography quantitative analysis, content of oleanolic acid is 98.7%.
Embodiment 3
A method for separating high-purity Oleanolic Acid from Tai Bai Aralia wood, comprises the following steps:
1) get Tai Bai Aralia wood rhizome dry product 1Kg, wash with water totally, dry, pulverize; Join 15L water boil 2.0 hours, the water cooking liquid that inclines, the dregs of a decoction divide refluxing extraction 3 times with 85% ethanol, and each ethanol consumption is 12L;
2) merge the gac that alcohol extract adds alcohol extract volume 1.0%, at 55 DEG C, stir decolouring 0.6 hour; Filtering gac, it is 11 left and right that decolouring alcohol extract regulates ethanol extract pH value with 0.8mol/L aqueous sodium hydroxide solution, leave standstill after 8 hours and filter, except precipitation, after impurity screening, filtrate is at 60 DEG C, vacuum tightness reaches 0.09Mpa and concentrates filtrate to 1/5 left and right (7L) that concentrates front volume, have a large amount of insolubless to separate out, filter, leaching insolubles is Oleanolic Acid crude product 7.8g;
3) Oleanolic Acid crude product 7.8g obtained above is washed with appropriate pure water, water-insoluble is analyzed dissolve with methanol with 80ml, after fully mixing, filters, and removes insolubles, obtains sample solution;
4) sample solution gradation is splined on to high pressure and prepares liquid phase and separate, chromatographic column is taking octadecylsilane chemically bonded silica as weighting agent, taking methanol-water system as elutriant; Detection wavelength is 210nm; With the speed isorheic elution 40min of 10ml/min, in described elutriant, the volume ratio of methyl alcohol and water is 93:7; Described gradation loading is each loading 10～20ml sample;
5) under detecting, UV-detector carries out Fractional Collections according to chromatogram appearance time, observe chromatographic peak by software, in the time that starting to rise, collects at the corresponding peak of Oleanolic Acid, on 9.4min Oleanolic Acid product peak, rise, collect by automatic fraction collector, collection time is that Oleanolic Acid peak starts ascent stage 9.45 minutes, and the peak whole peak height 1/5th that declines finishes to collect.After 30min, finish this elution system, carry out the collection of repetition sample introduction, until the Oleanolic Acid sample solution sample introduction of preparation is complete, collect liquid and in Rotary Evaporators, reclaim solvent, at 60 DEG C, vacuum tightness reaches 0.09Mpa, and olea acid solution is evaporated to without methyl alcohol taste, and precipitate can obtain highly purified Oleanolic Acid with the distilled water washing of boiling; Obtain dried powder 0.87g, by high performance liquid chromatography quantitative analysis, content of oleanolic acid is 98.3%.
To sum up, high performance preparative liquid chromatography provided by the present invention separates the method for Oleanolic Acid, under UV-detector on-line monitoring, carry out the accurate collection of separated product and impurity, sepn process simple and fast, flash liberation just can achieve the goal, and has effectively ensured that Oleanolic Acid can not lose, and the sepn process used time is short, fractional dose is large, and particularly purity can reach more than 98%.Present method running cost is low, and filler for a long time recirculation uses, and solvent is recyclable to be reused, and disengaging time is short, and fractional dose is large, is applicable to suitability for industrialized production.
Claims (10)
1. a method of preparing high purity oleanolic acid from too white Aralia wood, is characterized in that, comprises the following steps:
1) washing of will be too white Aralia wood Oleanolic Acid crude product, gets insolubles, according to 1g:(3～7) solid-liquid ratio of mL, in insolubles, add analysis methyl alcohol, fully mix, cross leaching supernatant, obtain sample solution;
2) fill after high pressure preparative liquid chromatography post with octadecylsilane chemically bonded silica, sample solution is splined on to high pressure preparative liquid chromatography post, taking methanol-water system as elutriant, with speed isorheic elution 30～40min of 10～200mL/min; In described elutriant, the volume ratio of methyl alcohol and water is (90～97): (10～3);
3) under detecting, UV-detector carries out Fractional Collections according to chromatogram appearance time, in the time that starting to rise, collects at the corresponding peak of Oleanolic Acid, when dropping to, this peak finishes five of whole peak height/a period of time to collect, obtain olea acid solution, olea acid solution is evaporated to without methyl alcohol taste, precipitate is washed with boiling water, obtains high purity oleanolic acid.
2. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 1, is characterized in that step 2) described loading employing gradation loading, each loading 10～20mL.
3. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 1, is characterized in that, the particle diameter of described octadecylsilane chemically bonded silica is 5～20 μ m; Column length 15～the 25cm of high pressure preparative liquid chromatography post; It is 210nm that described high pressure liquid chromatography post detects wavelength.
4. a kind of method of preparing high purity oleanolic acid from too white Aralia wood according to claim 1, is characterized in that step 3) described olea acid solution concentrating under reduced pressure is at 40～60 DEG C, under the condition that vacuum tightness is 0.09～0.15Mpa, carries out.
5. according to a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood described in any one in claim 1～4, it is characterized in that, the preparation of described Tai Bai Aralia wood Oleanolic Acid crude product comprises the following steps:
1) by pretreated too white Aralia wood medicinal material with filtering after water extraction, get filter residue, after the ethanolic soln refluxing extraction that is 85%～95% with massfraction by filter residue, filtration again, obtains ethanol extract;
2) by ethanol extract activated carbon decolorizing, then filtering gac, then regulate ethanol extract pH value to alkalescence, and filtering and impurity removing after leaving standstill, filters after filtrate decompression is concentrated again, and get is Dao Aralia wood Oleanolic Acid crude product.
6. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 5, is characterized in that, described pretreated Tai Bai Aralia wood medicinal material is that the stem skin of Tai Bai Aralia wood and root are obtained after washing, dry and pulverization process.
7. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 5, it is characterized in that, step 1) described with water extraction be by pretreated too white Aralia wood medicinal material use flooding three times, each 1～2h, wherein, the amount ratio of pretreated Tai Bai Aralia wood medicinal material and water is 1g:(10～15) mL; The number of times of described refluxing extraction is 2～3 times, each 1.5～2h, wherein, the amount ratio of the ethanolic soln that pretreated Tai Bai Aralia wood medicinal material and massfraction are 85%～95% is 1g:(8～12) mL.
8. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 5, is characterized in that step 2) be pH value to 9～11 that regulate ethanol extract with 0.5～1.0mol/L aqueous sodium hydroxide solution.
9. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 5, is characterized in that step 2) in the volume of filtrate decompression after concentrated be 1/3～1/5 of concentrated front volume; Concentrating under reduced pressure is at 40～60 DEG C, under the condition that vacuum tightness is 0.09～0.15Mpa, carries out.
10. a kind of method of preparing high purity oleanolic acid from Tai Bai Aralia wood according to claim 5, it is characterized in that, step 2) consumption of active carbon for decolorization is 0.1%～1.0% of ethanol extract volume, decolouring is at 50～70 DEG C, fully stirs 15～60min; Repeat to add activated carbon decolorizing to process 2～3 times.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478985A (en) * | 2014-11-20 | 2015-04-01 | 天津理工大学 | Method for extracting oleanolic acid from Japanese aralia leaves |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303850A (en) * | 1999-10-26 | 2001-07-18 | 上海长海医院 | Method for producing oleanolic acid |
| CN101735301A (en) * | 2009-12-15 | 2010-06-16 | 湖北香连药业有限责任公司 | Method for extracting high purity oleanolic acid |
| CN101857625A (en) * | 2009-11-18 | 2010-10-13 | 青海清华博众生物技术有限公司 | Method for extracting oleanolic acid from sea-buckthorn |
-
2014
- 2014-06-18 CN CN201410273605.8A patent/CN104031113A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303850A (en) * | 1999-10-26 | 2001-07-18 | 上海长海医院 | Method for producing oleanolic acid |
| CN101857625A (en) * | 2009-11-18 | 2010-10-13 | 青海清华博众生物技术有限公司 | Method for extracting oleanolic acid from sea-buckthorn |
| CN101735301A (en) * | 2009-12-15 | 2010-06-16 | 湖北香连药业有限责任公司 | Method for extracting high purity oleanolic acid |
Non-Patent Citations (1)
| Title |
|---|
| 田吉 等: "高效液相色谱法测定楤木及其提取物中齐墩果酸的含量", 《时珍国医国药》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478985A (en) * | 2014-11-20 | 2015-04-01 | 天津理工大学 | Method for extracting oleanolic acid from Japanese aralia leaves |
| CN104478985B (en) * | 2014-11-20 | 2016-04-06 | 天津理工大学 | A kind of method extracting Oleanolic Acid from this Aralia of wood blade |
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Application publication date: 20140910 |