CN102464698A - Preparation method of high-content echinocystic acid - Google Patents
Preparation method of high-content echinocystic acid Download PDFInfo
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- CN102464698A CN102464698A CN2010105497737A CN201010549773A CN102464698A CN 102464698 A CN102464698 A CN 102464698A CN 2010105497737 A CN2010105497737 A CN 2010105497737A CN 201010549773 A CN201010549773 A CN 201010549773A CN 102464698 A CN102464698 A CN 102464698A
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- YKOPWPOFWMYZJZ-FMMUPTMQSA-N Echinocystic acid Natural products C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)C[C@H](O)[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C YKOPWPOFWMYZJZ-FMMUPTMQSA-N 0.000 title claims abstract description 24
- YKOPWPOFWMYZJZ-UHFFFAOYSA-N Echinocystsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CC(O)C5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C YKOPWPOFWMYZJZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- MCHWKJRTMPIHRA-UHFFFAOYSA-N n-(pyrrolidin-2-ylmethyl)aniline Chemical compound C1CCNC1CNC1=CC=CC=C1 MCHWKJRTMPIHRA-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 241000931143 Gleditsia sinensis Species 0.000 claims abstract description 21
- 238000010992 reflux Methods 0.000 claims abstract description 20
- 238000000967 suction filtration Methods 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000007062 hydrolysis Effects 0.000 claims abstract description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 9
- 230000006837 decompression Effects 0.000 claims description 7
- 230000008030 elimination Effects 0.000 claims description 7
- 238000003379 elimination reaction Methods 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- 208000021302 gastroesophageal reflux disease Diseases 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract 4
- 239000000706 filtrate Substances 0.000 abstract 2
- 238000004042 decolorization Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000002045 lasting effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 230000008021 deposition Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229930182490 saponin Natural products 0.000 description 4
- 150000007949 saponins Chemical class 0.000 description 4
- 235000017709 saponins Nutrition 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 206010062717 Increased upper airway secretion Diseases 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 description 3
- 238000004440 column chromatography Methods 0.000 description 3
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 3
- 208000031225 myocardial ischemia Diseases 0.000 description 3
- 208000026435 phlegm Diseases 0.000 description 3
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- DKVBOUDTNWVDEP-NJCHZNEYSA-N teicoplanin aglycone Chemical compound N([C@H](C(N[C@@H](C1=CC(O)=CC(O)=C1C=1C(O)=CC=C2C=1)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)OC=1C=C3C=C(C=1O)OC1=CC=C(C=C1Cl)C[C@H](C(=O)N1)NC([C@H](N)C=4C=C(O5)C(O)=CC=4)=O)C(=O)[C@@H]2NC(=O)[C@@H]3NC(=O)[C@@H]1C1=CC5=CC(O)=C1 DKVBOUDTNWVDEP-NJCHZNEYSA-N 0.000 description 2
- -1 10L water-saturated n-butanol Chemical class 0.000 description 1
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- 206010008132 Cerebral thrombosis Diseases 0.000 description 1
- 206010008190 Cerebrovascular accident Diseases 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 201000001429 Intracranial Thrombosis Diseases 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 206010036790 Productive cough Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 208000006011 Stroke Diseases 0.000 description 1
- 208000003443 Unconsciousness Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- ZPHQBFRCXUIIAZ-UHFFFAOYSA-N benzene;hydrochloride Chemical compound Cl.C1=CC=CC=C1 ZPHQBFRCXUIIAZ-UHFFFAOYSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
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- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of high-content echinocystic acid. The process comprises the steps of crushing gleditsia sinensis, adding 5-8 times of 50-70% ethanol, performing heat preservation extraction for 2-3 times, each time lasting for 1-2 hours, adding 1-2% of activated carbon into an extracting solution for decolorization, filtering, recovering ethanol under reduced pressure, adding water saturated n-butanol into a concentrated solution for extraction for 2-4 times, collecting an n-butanol layer, adding hydrochloric acid for reflux hydrolysis for 2-3 hours, cooling, performing suction filtration on a precipitate, washing the precipitate to be neutral by deionized water, dissolving the precipitate by using 3-5 times of alkaline ethanol solution, filtering out insoluble substances, adjusting the pH of filtrate to 7-9 by using hydrochloric acid, filtering, adjusting the pH of the filtrate to 2-4, filtering out the precipitate, completely refluxing and dissolving and crystallizing the solid by using 70-90% ethanol for 2-3 times, and drying the crystal to obtain the. The method for producing the echinocystic acid has the advantages of simple process operation, high product content and no solvent residue.
Description
Technical field:
The invention belongs to natural plant field, particularly relate to a kind of preparation method of high-content Echinocystic acid.
Background technology:
Echinocystic acid is volatile oil property sapogenin, white needle (ethanol); Odorless, tasteless, be dissolved in methyl alcohol, ethanol, benzene, chloroform, water-soluble hardly.Echinocystic acid has function of resisting myocardial ischemia, is used to treat diseases such as coronary heart disease, stenocardia, cerebral thrombosis.
Chinese honey locust is pulse family Gleditsia officinalis fruit or sterile fruit.Having eliminates the phlegm has one's ideas straightened out, mass dissipating and swelling eliminating, and the merit of wind dispelling insecticide cures mainly apoplexy, remains unconscious, and insane pain phlegm is contained, and the pass key is obstructed, and stupid productive cough is breathed heavily, and it is not well to cough up phlegm, the disease of constipation due to dry stool.Mainly be to contain research bases such as quantitative relevant Chinese honey locust chemical ingredients, pharmacologically active in the Chinese honey locust.Modern medicine study shows that Chinese honey locust mainly contains saponins, triterpenes, flavonoid, phenolic acids, steroidal class material, has pharmacologically actives such as antibiotic, desinsection, anti-inflammatory, antitumor, resisting myocardial ischemia, antianaphylaxis.
Echinocystic acid in Chinese honey locust mainly be with glycoside exist with small portion be aglycon.The drug effect of glycosides can not show a candle to the aglycon effect.From Chinese honey locust, carrying Echinocystic acid is generally acid hydrolysis and makes.
Like patent " preparation method of Echinocystic acid, pharmaceutical prepn and new medical use "; This patent disclosed method is with the alcohol reflux of Chinese medicine Chinese honey locust with 70%-95%; Get total saponins through method purifying such as adjust pH or macroporous resin column chromatographies, the acid that adds finite concentration and volume again is hydrolyzed, purifying can get the pure article of Echinocystic acid.Document " Chinese honey locust activity against myocardial ischemia composition screening and mechanism research " for another example; The method that adopts is that this comprehensive study adopts separation means such as alcohol reflux, acid hydrolysis, normal phase column chromatography, reversed phase column chromatography to prepare Chinese honey locust total saponins and Chinese honey locust total sapogenin, and further Chinese honey locust total sapogenin chemical ingredients is separated.
Also have document " purifying of the total saponin of Chinese honey locust and assay ", the method for employing is a n-butanol extraction, ethyl acetate extraction, and silicagel column separates, the hydrolysis of hydrochloric acid benzole soln.
As stated, existing technological operation is loaded down with trivial details, and cost is higher.
Summary of the invention:
It is simple that the technical problem that the present invention will solve provides a kind of technological operation, the preparation method of the high-content Echinocystic acid that energy consumption is lower.
The objective of the invention is to realize like this:
A kind of preparation method of high-content Echinocystic acid is characterized in that may further comprise the steps: get Chinese honey locust and pulverize, add 5-8 and doubly measure 50-70% ethanol insulation extraction 2-3 time, each 1-2 hour; Extracting solution adds the 1-2% activated carbon decolorizing, filters, and decompression recycling ethanol, liquid concentrator add water-saturated n-butanol extraction 2-4 time; Collect n-butanol layer, add hydrochloric acid reflux hydrolysis 2-3 hour, cooling back suction filtration throw out, deionized water wash is to neutral; Throw out is doubly measured the alkaline ethanol solution dissolving with 3-5, the elimination insolubles, and filtrating hydrochloric acid is regulated pH7-9; Filter, filtrating re-adjustment pH2-4 leaches throw out; Solids is used dissolving crystallized 2-3 time of 70-90% ethanol total reflux again, the dry Echinocystic acid product that gets of crystallisate, and content is not less than 95%.
50-60 ℃ of temperature extracted in said insulation.
The hydrochloric acid consumption is hydrochloric 2-4mol/L in the liquid in the said hydrolysis.
Said alkaline ethanol is the 50-70% aqueous ethanolic solution that contains 1-2% Pottasium Hydroxide or sodium hydroxide.
Present method positively effect is: first extraction using alcohol activated carbon decolorizing, and more simple to operate than follow-up activated carbon decolorizing, can thoroughly remove gac at alkali alcohol dissolution process, because the activated carbon granule inequality is easy to remain in the product; Acid hydrolysis in the propyl carbinol can be saved macroporous resin adsorption, reduces the crystallization number of times; The dissolving of alkali alcohol, different pH good impurity removing effect, simple to operate.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get Chinese honey locust and pulverize, get 2kg, add 60 ℃ of insulations of 16L50% ethanol heating 2 hours, suction filtration liquid; Added the 10L50% extraction using alcohol again 1 hour, united extraction liquid adds 140g gac reflux decolour 1 hour, filtering gac, destainer decompression recycling ethanol; Liquid concentrator adds the 200ml water-saturated n-butanol and fully stirs, and collects n-butanol layer after the layering, adds 100ml water-saturated n-butanol extraction 2 times again, collects n-butanol layer; Add hydrochloric acid, make its concentration reach 2mol/L, back hydrolysis 3 hours, cooling back suction filtration throw out; Deionized water wash is to neutral, and throw out is with 5 times of amount 50% ethanolic solns (containing 1% sodium hydroxide) dissolving, elimination insolubles; Filtrating hydrochloric acid is regulated pH8, filters filtrating re-adjustment pH3 deposition; Leach throw out with 90% alcohol reflux dissolving crystallized for 2 times, crystallisate dry needle-like white crystal Echinocystic acid, content detection 96.5%.
Embodiment 2:
Get Chinese honey locust and pulverize, get 2kg, add 50 ℃ of insulations of 16L70% ethanol heating 2 hours, suction filtration liquid; Added the 10L70% extraction using alcohol again 1 hour, united extraction liquid adds 200g gac reflux decolour 1 hour, filtering gac, destainer decompression recycling ethanol; Liquid concentrator adds the 100ml water-saturated n-butanol and fully stirs, and collects n-butanol layer after the layering, adds 100ml water-saturated n-butanol extraction 3 times again, collects n-butanol layer; Add hydrochloric acid, make its concentration reach 4mol/L, back hydrolysis 2 hours, cooling back suction filtration throw out; Deionized water wash is to neutral, and throw out dissolves with 3 times of amount 70% ethanolic solns (containing 2% sodium hydroxide), the elimination insolubles, and filtrating hydrochloric acid is regulated pH7; Filter, filtrating re-adjustment pH2 deposition, it is dissolving crystallized with 70% alcohol reflux to leach throw out; Use 90% alcohol reflux dissolving crystallized again, dry needle-like white crystal Echinocystic acid, the content detection 97.1% of getting of crystallisate.
Embodiment 3:
Get Chinese honey locust and pulverize, get 4kg, add 50 ℃ of insulations of 32L70% ethanol heating 2 hours, suction filtration liquid; Added the 32L70% extraction using alcohol again 1 hour, united extraction liquid adds 400g gac reflux decolour 1 hour, filtering gac, destainer decompression recycling ethanol; Liquid concentrator adds the 500ml water-saturated n-butanol and fully stirs, and collects n-butanol layer after the layering, adds the extraction of 500ml water-saturated n-butanol again, collects n-butanol layer; Add hydrochloric acid, make its concentration reach 2mol/L, back hydrolysis 3 hours, cooling back suction filtration throw out; Deionized water wash is to neutral, and throw out dissolves with 4 times of amount 60% ethanolic solns (containing 2% Pottasium Hydroxide), the elimination insolubles, and filtrating hydrochloric acid is regulated pH8; Filter, filtrating re-adjustment pH3 deposition, it is dissolving crystallized with 80% alcohol reflux to leach throw out; Use 90% alcohol reflux dissolving crystallized again, dry needle-like white crystal Echinocystic acid, the content detection 96.5% of getting of crystallisate.
Embodiment 4:
Get Chinese honey locust and pulverize, get 10kg, add 50 ℃ of insulations of 60L70% ethanol heating 2 hours, suction filtration liquid; Add the 50L70% extraction using alcohol again 2 times, united extraction liquid adds 800g gac reflux decolour 1 hour, filtering gac, destainer decompression recycling ethanol; Liquid concentrator adds the 1L water-saturated n-butanol and fully stirs, and collects n-butanol layer after the layering, adds 1L water-saturated n-butanol extraction 2 times again, collects n-butanol layer; Add hydrochloric acid, make its concentration reach 2mol/L, back hydrolysis 3 hours, cooling back suction filtration throw out; Deionized water wash is to neutral, and throw out dissolves with 4 times of amount 60% ethanolic solns (containing 1% Pottasium Hydroxide), the elimination insolubles, and filtrating hydrochloric acid is regulated pH8; Filter, filtrating re-adjustment pH3 deposition, it is dissolving crystallized with 80% alcohol reflux to leach throw out; Use 90% alcohol reflux dissolving crystallized again, dry needle-like white crystal Echinocystic acid, the content detection 95.8% of getting of crystallisate.
Embodiment 5:
Get Chinese honey locust and pulverize, get 100kg, add 50 ℃ of insulations of 600L70% ethanol heating 2 hours, suction filtration liquid; Add the 500L70% extraction using alcohol again 2 times, united extraction liquid adds 8000g gac reflux decolour 1 hour, filtering gac, destainer decompression recycling ethanol; Liquid concentrator adds the 10L water-saturated n-butanol and fully stirs, and collects n-butanol layer after the layering, adds the equivalent n-butanol extraction again 2 times, collects n-butanol layer; Add hydrochloric acid, make its concentration reach 2mol/L, back hydrolysis 3 hours, cooling back suction filtration throw out; Deionized water wash is to neutral, and throw out dissolves with 4 times of amount 70% ethanolic solns (containing 2% Pottasium Hydroxide), the elimination insolubles, and filtrating hydrochloric acid is regulated pH8; Filter, filtrating re-adjustment pH4 deposition, it is dissolving crystallized with 70% alcohol reflux to leach throw out; Use 90% alcohol reflux dissolving crystallized again, dry needle-like white crystal Echinocystic acid, the content detection 96.5% of getting of crystallisate.
Claims (4)
1. the preparation method of a high-content Echinocystic acid is characterized in that may further comprise the steps: get Chinese honey locust and pulverize, add 5-8 and doubly measure 50-70% ethanol insulation extraction 2-3 time, each 1-2 hour; Extracting solution adds the 1-2% activated carbon decolorizing, filters, and decompression recycling ethanol, liquid concentrator add water-saturated n-butanol extraction 2-4 time; Collect n-butanol layer, add hydrochloric acid reflux hydrolysis 2-3 hour, cooling back suction filtration throw out, deionized water wash is to neutral; Throw out is doubly measured the alkaline ethanol solution dissolving with 3-5, the elimination insolubles, and filtrating hydrochloric acid is regulated pH7-9; Filter, filtrating re-adjustment pH2-4 leaches throw out; Solids is used dissolving crystallized 2-3 time of 70-90% ethanol total reflux again, the dry Echinocystic acid product that gets of crystallisate, and content is not less than 95%.
2. according to the preparation method of the said high-content Echinocystic acid of claim 1, it is characterized in that 50-60 ℃ of said insulation extraction temperature.
3. according to the preparation method of the said high-content Echinocystic acid of claim 1, it is characterized in that concentration of hydrochloric acid is 2-4mol/L in the said hydrolysis.
4. according to the preparation method of the said high-content Echinocystic acid of claim 1, it is characterized in that said alkaline ethanol is the 50-70% aqueous ethanolic solution that contains 1-2% Pottasium Hydroxide or sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105497737A CN102464698A (en) | 2010-11-19 | 2010-11-19 | Preparation method of high-content echinocystic acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105497737A CN102464698A (en) | 2010-11-19 | 2010-11-19 | Preparation method of high-content echinocystic acid |
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| CN102464698A true CN102464698A (en) | 2012-05-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103083388A (en) * | 2012-12-31 | 2013-05-08 | 山东省中医药研究院 | Preparation method of fructus gleditsiae total saponins |
| CN109549942A (en) * | 2019-01-16 | 2019-04-02 | 于海龙 | Application of the echinocystic acid in treatment cerebral infarction medicine preparation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438237A (en) * | 2003-01-21 | 2003-08-27 | 吉林天药科技股份有限公司 | Echinocystic acid preparation, medicinal preparation and new use as medicine |
| CN101884637A (en) * | 2009-05-15 | 2010-11-17 | 成都康弘制药有限公司 | Medicinal composition for treating cardiovascular diseases and application thereof |
-
2010
- 2010-11-19 CN CN2010105497737A patent/CN102464698A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438237A (en) * | 2003-01-21 | 2003-08-27 | 吉林天药科技股份有限公司 | Echinocystic acid preparation, medicinal preparation and new use as medicine |
| CN101884637A (en) * | 2009-05-15 | 2010-11-17 | 成都康弘制药有限公司 | Medicinal composition for treating cardiovascular diseases and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 姚新生: "《天然药物化学》", 30 June 2001, article "天然药物化学", pages: 332 - 18 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103083388A (en) * | 2012-12-31 | 2013-05-08 | 山东省中医药研究院 | Preparation method of fructus gleditsiae total saponins |
| CN103083388B (en) * | 2012-12-31 | 2015-07-01 | 山东省中医药研究院 | Preparation method of fructus gleditsiae total saponins |
| CN109549942A (en) * | 2019-01-16 | 2019-04-02 | 于海龙 | Application of the echinocystic acid in treatment cerebral infarction medicine preparation |
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