CN102464698A - Method for preparing high-content echinocystic acid - Google Patents
Method for preparing 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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Abstract
The invention relates to a method for preparing high-content echinocystic acid, which comprises the following process steps: taking honey locust to be crushed, adding 50-70% ethanol of which the amount is 5-8 times larger than that of the honey locust for extraction for 2-3 times at a constant temperature for 1-2 hours each time, adding 1-2% active carbon to an extract for decoloring, filtering, recovering ethanol by decompression; adding water-saturated n-butanol to a concentrated solution for extraction for 2-4 times, collecting an n-butanol layer, and adding hydrochloric acid for reflux hydrolysis for 2-3 hours; after cooling, leaching sediments, washing with deionized water to be neutral, allowing the sediments to be dissolved with an alkaline ethanol solution of which the amount is 3-5 times larger than that of the sediments, and filtering out insolubles; adjusting the pH value of a filtrate to be between 7 and 9 with the hydrochloric acid, filtering, and then adjusting the pH value of the filtrate to be between 2 and 4; and filtering out the sediments, carrying complete reflux, dissolution and crystallization of a solid with 70-90% ethanol for 2-3 times, and drying crystals to obtain the echinocystic acid with the content of not less than 95%. According to the method for producing the echinocystic acid in the invention, the process operation is simple, the product content is high, and residual solvents do not exist.
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.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105497737A CN102464698A (en) | 2010-11-19 | 2010-11-19 | Method for preparing high-content echinocystic acid |
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| CN2010105497737A CN102464698A (en) | 2010-11-19 | 2010-11-19 | Method for preparing 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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Application publication date: 20120523 |