CN103242396A - Method for preparing sec-o-glucosylhamaudol - Google Patents
Method for preparing sec-o-glucosylhamaudol Download PDFInfo
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- CN103242396A CN103242396A CN2013101793561A CN201310179356A CN103242396A CN 103242396 A CN103242396 A CN 103242396A CN 2013101793561 A CN2013101793561 A CN 2013101793561A CN 201310179356 A CN201310179356 A CN 201310179356A CN 103242396 A CN103242396 A CN 103242396A
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- methanol solution
- under reduced
- reduced pressure
- glycosides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses an efficient, simple and convenient method for preparing sec-o-glucosylhamaudol. The method comprises the following steps of: crushing Chinese parsnip root; adding 40 to 70 percent methanol solution and performing ultrasonic extraction for 2 to 3 times; concentrating the extracted liquid until the concentrated liquid does not contain methanol; adding polyamide resin for adsorbing; performing gradient elution with methanol solution; collecting the eluted solution and concentrating the eluted solution under reduced pressure; separating and purifying the concentrated solution by using a high-speed counter current chromatograph; monitoring by using an ultraviolet detector online; collecting the fraction; and drying the fraction under reduced pressure to obtain sec-o-glucosylhamaudol. According to the method, the process operation is simple, the product yield is high, the reagent can be recycled, and the method is applicable to prepare high-purity sec-o-glucosylhamaudol.
Description
Technical field
The separating and purifying technology field of pharmaceutically active ingredient is specifically related to a kind of method for preparing the hamaudol glycosides in the invention belongs to.
Background technology
The hamaudol glycosides is polyphenols, CAS 80681-44-3, molecular formula C
21H
26O
10, molecular weight 438.42, molecular structural formula:
Windproof is the root of umbelliferae Saposhnikovia divaricata, is one of China's large medicinal material commonly used, has inducing diaphoresis to dispel wind, wins and wet, end the convulsion function, is used for treatments such as flu headache, rheumatic arthralgia, rubella itch, tetanus.The activeconstituents that windproof garment is wanted is chromogen ketones such as macrotin glycosides, macrotin, 5-O-methyl visamminol glycosides and hamaudol glycosides and polysaccharide, coumarins etc.Modern pharmacological research shows that windproof chromone has multiple efficacies such as analgesic, analgesia, anti-inflammatory, antitumor, platelet aggregation-against, is used for the treatment of cerebral concussion, infantile respiratory tract infection, allergic dermatitis, facial neuritis, toothache etc.The method for preparing the hamaudol glycosides by literature search from windproof is less.(application number: 201010603919.1) " a kind of separation purification method of hamaudol glycosides " provides the method for the separation and purification hamaudol glycosides from windproof chromone extractive by macroporous resin adsorption and gel filtration chromatography method as patent.Utilize the shortcoming of silicagel column or gel column separation and purification to be, sample loss is more, and reagent dosage is big, and the solvent gradient is more, is not easy control, and technology is loaded down with trivial details.
Summary of the invention
The objective of the invention is to overcome defective and the deficiency of prior art, a kind of efficient, short-cut method for preparing the hamaudol glycosides is provided.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method for preparing the hamaudol glycosides, it is characterized in that: with windproof pulverizing medicinal materials, add 40-70% methanol solution supersound extraction 2-3 time, extracting solution is concentrated into does not have alcohol, adds polyamide resin absorption, the methanol solution gradient elution, collect the elutriant concentrating under reduced pressure, the gained concentrated solution adopts the high-speed counter-current chromatograph separation and purification again, the UV-detector on-line monitoring, collect flow point, drying under reduced pressure namely.
Described methanol solution gradient elution is: 3-5 times of column volume 20-40% methanol solution wash-out impurity, and again with 4-7 times of column volume 40-60% methanol solution wash-out effective constituent.
Described high-speed counter-current chromatograph separation and purification solvent systems is: propyl carbinol, ethyl acetate, water, according to the 3:5:7 mixed, fully mix, and take off and do moving phase mutually, get the phase that fixes mutually.
Utilize present method to prepare the hamaudol glycosides, technological operation is simple, yield is high, products obtained therefrom purity height.
Embodiment:
Be described further below with reference to the invention of embodiment, but do not limit the scope of the invention.
Embodiment 1:
Get the windproof medicinal material of 5kg, use 30L60% methyl alcohol supersound extraction 3 times, each 30 minutes, extracting solution merges concentrating under reduced pressure, and concentrated solution adds in the 2L polyamide resin column and adsorbs, earlier with 8L30% methanol solution wash-out impurity, use 10L50% methanol solution wash-out again, collect the elutriant concentrating under reduced pressure and get medicinal extract.Get propyl carbinol, ethyl acetate, water, according to the 3:5:7 mixed, fully mix, getting fixes mutually injects the high speed adverse current chromatogram pipe mutually, drives alternation of hosts's machine, velocity of rotation 800rpm, pump into down simultaneously and do moving phase mutually, after the system balancing, flow rate regulation is 2ml/min, dissolve medicinal extract with moving phase, by the sampling valve sample introduction, according to the UV-detector collection of illustrative plates, collect flow point, preparation continuously, flow point merge the dry brown powder 1.2g of getting of concentrating under reduced pressure, content 98.3%.
Embodiment 2:
Get the windproof medicinal material of 5kg, use 40L50% methyl alcohol supersound extraction 2 times, each 30 minutes, extracting solution merges concentrating under reduced pressure, and concentrated solution adds in the 2L polyamide resin column and adsorbs, earlier with 10L20% methanol solution wash-out impurity, use 8L55% methanol solution wash-out again, collect the elutriant concentrating under reduced pressure and get medicinal extract.Get propyl carbinol, ethyl acetate, water, according to the 3:5:7 mixed, fully mix, getting fixes mutually injects the high speed adverse current chromatogram pipe mutually, drives alternation of hosts's machine, velocity of rotation 900rpm, pump into down simultaneously and do moving phase mutually, after the system balancing, flow rate regulation is 3ml/min, dissolve medicinal extract with moving phase, by the sampling valve sample introduction, according to the UV-detector collection of illustrative plates, collect flow point, preparation continuously, flow point merge the dry brown powder 1.3g of getting of concentrating under reduced pressure, and content 98.7% is implemented
Embodiment 3:
Get the windproof medicinal material of 5kg, use 30L60% methyl alcohol supersound extraction 3 times, each 30 minutes, extracting solution merges concentrating under reduced pressure, and concentrated solution adds in the 2L polyamide resin column and adsorbs, earlier with 8L25% methanol solution wash-out impurity, use 14L45% methanol solution wash-out again, collect the elutriant concentrating under reduced pressure and get medicinal extract.Get propyl carbinol, ethyl acetate, water, according to the 3:5:7 mixed, fully mix, getting fixes mutually injects the high speed adverse current chromatogram pipe mutually, drives alternation of hosts's machine, velocity of rotation 850rpm, pump into down simultaneously and do moving phase mutually, after the system balancing, flow rate regulation is 1ml/min, dissolve medicinal extract with moving phase, by the sampling valve sample introduction, according to the UV-detector collection of illustrative plates, collect flow point, preparation continuously, flow point merge the dry brown powder 1.5g of getting of concentrating under reduced pressure, content 97.4%.
Claims (3)
1. method for preparing the hamaudol glycosides, it is characterized in that: with windproof pulverizing medicinal materials, add 40-70% methanol solution supersound extraction 2-3 time, extracting solution is concentrated into does not have alcohol, adds polyamide resin absorption, the methanol solution gradient elution, collect the elutriant concentrating under reduced pressure, the gained concentrated solution adopts the high-speed counter-current chromatograph separation and purification again, the UV-detector on-line monitoring, collect flow point, drying under reduced pressure namely.
2. according to the described method for preparing the hamaudol glycosides of claim 1, it is characterized in that described methanol solution gradient elution is: 3-5 times of column volume 20-40% methanol solution wash-out impurity, again with 4-7 times of column volume 40-60% methanol solution wash-out effective constituent.
3. according to the described method for preparing the hamaudol glycosides of claim 1, it is characterized in that described high-speed counter-current chromatograph separation and purification solvent systems is: propyl carbinol, ethyl acetate, water, according to the 3:5:7 mixed, fully mix, take off and do moving phase mutually, get the phase that fixes mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101793561A CN103242396A (en) | 2013-05-15 | 2013-05-15 | Method for preparing sec-o-glucosylhamaudol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101793561A CN103242396A (en) | 2013-05-15 | 2013-05-15 | Method for preparing sec-o-glucosylhamaudol |
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| CN103242396A true CN103242396A (en) | 2013-08-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2013101793561A Pending CN103242396A (en) | 2013-05-15 | 2013-05-15 | Method for preparing sec-o-glucosylhamaudol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107864860A (en) * | 2017-12-06 | 2018-04-03 | 赵腾骅 | A kind of cultural method for improving sec-o-glucosylhamaudol content in windproof callus |
| CN113189256A (en) * | 2021-05-12 | 2021-07-30 | 劲牌有限公司 | Method for extracting curculigoside from curculigo orchioides |
-
2013
- 2013-05-15 CN CN2013101793561A patent/CN103242396A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107864860A (en) * | 2017-12-06 | 2018-04-03 | 赵腾骅 | A kind of cultural method for improving sec-o-glucosylhamaudol content in windproof callus |
| CN107864860B (en) * | 2017-12-06 | 2019-02-12 | 广州今成生物科技有限公司 | A kind of cultural method improving sec-o-glucosylhamaudol content in windproof callus |
| CN113189256A (en) * | 2021-05-12 | 2021-07-30 | 劲牌有限公司 | Method for extracting curculigoside from curculigo orchioides |
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Application publication date: 20130814 |