CN101602727A - A kind of preparation method of selagine - Google Patents
A kind of preparation method of selagine Download PDFInfo
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- CN101602727A CN101602727A CNA2009100272452A CN200910027245A CN101602727A CN 101602727 A CN101602727 A CN 101602727A CN A2009100272452 A CNA2009100272452 A CN A2009100272452A CN 200910027245 A CN200910027245 A CN 200910027245A CN 101602727 A CN101602727 A CN 101602727A
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- selagine
- chloroform
- exchange resin
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Abstract
The present invention relates to a kind of easy and simple to handle, preparation method of polluting little selagine, processing step is for getting the dry meal of Herba Lycopodii serrati, add 2-30 and doubly measure the acid solution supersound extraction, power 100-2000W, extracted 10-30 minute, and filtered, cross anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the macroporous adsorptive resins, the water elution removal of impurities, use the 50-90% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform crystallization, wash, be drying to obtain.Adopt the present invention to prepare selagine, the product purity height is easy to realize the industrialization amplification.
Description
Technical field
The present invention relates to a kind of preparation method of selagine, especially a kind of method of from plant, extracting selagine.
Background technology
Selagine (Huperzine A) is a kind of alkaloid that extracts from Chinese endemic plant Herba Lycopodii serrati (Herba Lycopodii serrati), it is a kind of world-class new drug of China's original creation, belonging to the reversibility anticholinesterase, is to treat benign memory deficits and degenerative brain disorder one of safe and effective medicine the most at present.
In the prior art, selagine mainly adopts the solvent method, and a large amount of soda acids that use are seriously polluted in the production process, and the production cycle is long, the production cost height, and the product yield is low, purity is low.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, selagine that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the dry meal of Herba Lycopodii serrati, add 2-30 and doubly measure the acid solution supersound extraction, power 100-2000W, extracted 10-30 minute, and filtered, cross anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, join on the macroporous adsorptive resins, the 50-90% ethanol elution is used in the water elution removal of impurities, collect elutriant, decompression recycling ethanol adds acetone-chloroform crystallization, washs, is drying to obtain.
Acid solution is selected from a kind of in 1% hydrochloric acid soln, 1% tartaric acid solution.
The supersound extraction condition is: add 20 times of amount acid solution supersound extraction, power 600W extracted 20 minutes.
Resin anion(R.A) is selected from a kind of in 201 * 2 type anionite-exchange resin, 201 * 4 type anionite-exchange resin, 201 * 7 type anionite-exchange resin, 330 type anionite-exchange resin, 321 type anionite-exchange resin, the 331 type anionite-exchange resin.
The model of macroporous adsorbent resin is a kind of among AB-8, H-103, the D-101.
The wash-out alcohol concn is 70%.
Crystallization is 1: 1 with the ratio of acetone-chloroform.
Adopt technique scheme to prepare selagine, easy and simple to handle, pollution is lacked, and is beneficial to big production operation.
Below in conjunction with embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get the dry meal 10Kg of Herba Lycopodii serrati, add 2 times of amount 1% tartaric acid solution supersound extraction, power 100W, extracted 10 minutes, and filtered, cross 201 * 2 type anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the AB-8 macroporous adsorptive resins, the water elution removal of impurities, use 50% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform (1: 1) crystallization, wash, be drying to obtain selagine 1.6g, detect through HPLC, purity is 95.2%.
Embodiment 2
Get the dry meal 10Kg of Herba Lycopodii serrati, add 30 times of amount 1% hydrochloric acid soln supersound extraction, power 2000W, extracted 30 minutes, and filtered, cross 201 * 4 type anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the H-103 macroporous adsorptive resins, the water elution removal of impurities, use 90% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform (1: 1) crystallization, wash, be drying to obtain selagine 3.4g, detect through HPLC, purity is 94.4%.
Embodiment 3
Get the dry meal 10Kg of Herba Lycopodii serrati, add 20 times of amount 1% tartaric acid solution supersound extraction, power 600W, extracted 20 minutes, and filtered, cross 201 * 7 type anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the D-101 macroporous adsorptive resins, the water elution removal of impurities, use 70% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform (1: 1) crystallization, wash, be drying to obtain selagine 2.4g, detect through HPLC, purity is 98.6%.
Embodiment 4
Get the dry meal 10Kg of Herba Lycopodii serrati, add 20 times of amount 1% tartaric acid solution supersound extraction, power 600W, extracted 20 minutes, and filtered, cross 330 type anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the D-101 macroporous adsorptive resins, the water elution removal of impurities, use 70% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform (2: 1) crystallization, wash, be drying to obtain selagine 1.6g, detect through HPLC, purity is 93.8%.
Embodiment 5
Get the dry meal 10Kg of Herba Lycopodii serrati, add 20 times of amount 1% tartaric acid solution supersound extraction, power 600W, extracted 20 minutes, and filtered, cross 321 type anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the D-101 macroporous adsorptive resins, the water elution removal of impurities, use 70% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform (1: 2) crystallization, wash, be drying to obtain selagine 1.8g, detect through HPLC, purity is 93.3%.
Embodiment 6
Get the dry meal 10Kg of Herba Lycopodii serrati, add 20 times of amount 1% tartaric acid solution supersound extraction, power 600W, extracted 20 minutes, and filtered, cross 331 type anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the D-101 macroporous adsorptive resins, the water elution removal of impurities, use 70% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform (1: 3) crystallization, wash, be drying to obtain selagine 1.1g, detect through HPLC, purity is 92.9%.
Claims (7)
1, a kind of preparation method of selagine, it is characterized in that described method comprises the following steps: to get the dry meal of Herba Lycopodii serrati, add 2-30 and doubly measure the acid solution supersound extraction, power 100-2000W, extracted 10-30 minute, and filtered, cross anionite-exchange resin, the soup chloroform extraction, the combined chloroform layer, the reclaim under reduced pressure chloroform also concentrates, and joins on the macroporous adsorptive resins, the water elution removal of impurities, use the 50-90% ethanol elution, collect elutriant, decompression recycling ethanol, add acetone-chloroform crystallization, wash, be drying to obtain.
2, the preparation method of a kind of selagine according to claim 1 is characterized in that described acid solution is selected from a kind of in 1% hydrochloric acid soln, 1% tartaric acid solution.
3, the preparation method of a kind of selagine according to claim 1 is characterized in that described supersound extraction condition is: add 20 times of amount acid solution supersound extraction, power 600W extracted 20 minutes.
4, the preparation method of a kind of selagine according to claim 1 is characterized in that described resin anion(R.A) is selected from a kind of in 201 * 2 type anionite-exchange resin, 201 * 4 type anionite-exchange resin, 201 * 7 type anionite-exchange resin, 330 type anionite-exchange resin, 321 type anionite-exchange resin, the 331 type anionite-exchange resin.
5, the preparation method of a kind of selagine according to claim 1, the model that it is characterized in that described macroporous adsorbent resin are a kind of among AB-8, H-103, the D-101.
6, the preparation method of a kind of selagine according to claim 1 is characterized in that described wash-out alcohol concn is 70%.
7, the preparation method of a kind of selagine according to claim 1, the ratio that it is characterized in that described acetone-chloroform is 1: 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009100272452A CN101602727A (en) | 2009-05-26 | 2009-05-26 | A kind of preparation method of selagine |
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| CNA2009100272452A CN101602727A (en) | 2009-05-26 | 2009-05-26 | A kind of preparation method of selagine |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491946A (en) * | 2011-12-12 | 2012-06-13 | 杭州华东医药集团康润制药有限公司 | Method for separating and purifying huperzine by molecular imprinting technology |
| CN102702101A (en) * | 2012-05-23 | 2012-10-03 | 长沙市惠瑞生物科技有限公司 | Method for extracting huperzine A from huperzine serrate |
| CN102977210A (en) * | 2012-11-16 | 2013-03-20 | 福建中医药大学 | Monoclonal antibody preparation method of huperzine A and enzyme-linked immune detection kit thereof |
| CN103951618A (en) * | 2014-05-09 | 2014-07-30 | 自贡天健生物科技有限公司 | Huperzine A crystal, and preparation method and application thereof |
| CN104016918A (en) * | 2012-03-22 | 2014-09-03 | 中国科学院上海药物研究所 | Huperzine A polymorphism body, preparation method thereof, pharmaceutical composition comprising polymorphism body and application thereof |
| JP2016527219A (en) * | 2013-07-15 | 2016-09-08 | 浙江万邦▲薬業▼股▲ふん▼有限公司Ｚｈｅｊｉａｎｇ Ｗａｎｂａｎｇ Ｐｈａｒｍａｃｅｕｔｉｃａｌ Ｐｌｃ． | Preparation of (-)-Huperzine A |
| CN106349162A (en) * | 2016-08-26 | 2017-01-25 | 安徽省虹升生物股份有限公司 | Method for extracting huperzine A from leaves of huperzia serrata |
-
2009
- 2009-05-26 CN CNA2009100272452A patent/CN101602727A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491946A (en) * | 2011-12-12 | 2012-06-13 | 杭州华东医药集团康润制药有限公司 | Method for separating and purifying huperzine by molecular imprinting technology |
| CN104016918A (en) * | 2012-03-22 | 2014-09-03 | 中国科学院上海药物研究所 | Huperzine A polymorphism body, preparation method thereof, pharmaceutical composition comprising polymorphism body and application thereof |
| CN104016918B (en) * | 2012-03-22 | 2016-04-13 | 中国科学院上海药物研究所 | Huperzine A polymorph, its preparation method, comprise the medical composition and its use of described polymorphs body |
| CN102702101A (en) * | 2012-05-23 | 2012-10-03 | 长沙市惠瑞生物科技有限公司 | Method for extracting huperzine A from huperzine serrate |
| CN102702101B (en) * | 2012-05-23 | 2016-04-06 | 长沙市惠瑞生物科技有限公司 | A kind of method extracting selagine from Herba Lycopodii serrati |
| CN102977210A (en) * | 2012-11-16 | 2013-03-20 | 福建中医药大学 | Monoclonal antibody preparation method of huperzine A and enzyme-linked immune detection kit thereof |
| JP2016527219A (en) * | 2013-07-15 | 2016-09-08 | 浙江万邦▲薬業▼股▲ふん▼有限公司Ｚｈｅｊｉａｎｇ Ｗａｎｂａｎｇ Ｐｈａｒｍａｃｅｕｔｉｃａｌ Ｐｌｃ． | Preparation of (-)-Huperzine A |
| CN103951618A (en) * | 2014-05-09 | 2014-07-30 | 自贡天健生物科技有限公司 | Huperzine A crystal, and preparation method and application thereof |
| CN106349162A (en) * | 2016-08-26 | 2017-01-25 | 安徽省虹升生物股份有限公司 | Method for extracting huperzine A from leaves of huperzia serrata |
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Application publication date: 20091216 |