Huperzine A production method suitable for industrial production

A technology for huperzine A and raw materials, which is applied in the field of industrial production of high-purity huperzine A, can solve the problems of affecting the curative effect, limited treatment amount, low yield and the like, and achieves product safety and environmental protection, water resources conservation, and simple operation. Effect

Inactive Publication Date: 2016-09-21
JIANGXI HAIFU BIOENG
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

At present, huperzine A has a good therapeutic effect on this type of disease in the world, and there are many pharmacological and toxicological studies on huperzine A abroad, but there is almost no separation and purification of huperzine A. For the purification and separation of huperzine A, solvent extraction is more used for separation, and there are more solvent residues, which affect the curative effect
[0004] CN 102617469A discloses a method for extracting huperzine A of Melaleuca, which comprises pulverizing the medicinal material of Melaleuca, ultrasonically extracting with acid solution, concentrating, adjusting pH with ammonia water, extracting with chloroform, dissolving acid solution again, and filtering with activated carbon for impurity removal , secondary ammonia water to adjust the pH value, chloroform extraction again, crystallization and recrystallization, and finally the product is dried. The purity of huperzine A in the product reaches 99%, and the yield of huperzine A is about 0.016%. Due to the process of repeated extraction , large loss, low yield and high cost
CN101693689A discloses a new method for extracting and separating high-purity huperzine A from the Melaleuca Tower. The method is to properly pulverize the medicinal material of the Melaleuca Tower, extract it with acid water, adjust the pH with ammonia water, absorb and separate the macroporous resin, and high-speed countercurrent Chromatographic purification, concentration and drying to obtain the finished product, the purity of huperzine A in the finished product can reach more than 98%, but in the process of this method, the investment of high-speed countercurrent chromatography equipment is large and the processing capacity is limited, so it is difficult to adapt to industrial production
CN 101602727A discloses a preparation method of huperzine A. The method is to use acid liquid to extract the coarse powder of the melaleuca tower, and prepare huperzine A with a purity of 90% through ion exchange, macroporous resin adsorption separation, crystallization and recrystallization. % more than the product, although the technique of this method is simple, operability is strong, but yield is unsatisfactory
CN102491946 A discloses a method for separating and purifying huperzine A by molecular imprinting technology. In this method, ultrasonic countercurrent extraction is carried out on the melaleuca medicinal material, and after concentration and decolorization, molecular imprinting polymerization, crystallization and recrystallization can prepare huperzine A with a purity of 99%. For the above products, the inventive method directly carries out ultrasonic countercurrent extraction of medicinal materials. Since the content of active ingredients in the Melaleuca tower is extremely low, there are many impurities extracted, which hinders the transfer of active substances in the solvent to a certain extent and affects the extraction yield of huperzine A. , which is unfavorable to the purification of subsequent processes; in addition, the molecular imprinting technology used in this method has high operability requirements, complicated control, and immature technology, which is only suitable for small batch production and is not conducive to scale-up and industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Pretreatment of raw materials: 400kg of the raw materials of the Melaleuca tower from which impurities have been separated are crushed with a pulverizer, and 100kg of raw materials that meet the process requirements are taken, and the content of huperzine A is 0.028%.

[0029] 2) Extraction: Put the crushed raw materials into the cleaned extraction tank, add 1100kg of 36°C, PH2.7 acid water for soaking and extraction, set the extraction time to 4h, stir and circulate for 10 minutes every 30 minutes; the first time After the extraction was completed, repeat three times, and all the extracts were combined (because of the test, the fourth extract was not applied).

[0030] 3) Centrifugation: The extract obtained in step (2) was centrifuged with a decanter centrifuge, and then passed through a disc centrifuge to obtain 3958 kg of centrifuge, and the temperature of the feed liquid was 37°C.

[0031] 4) Ultrafiltration: Pass the centrifugate obtained in step (3) through an...

Embodiment 2

[0037] 1) Pretreatment of raw materials: Take 100kg of raw materials that meet the process requirements, and the content of huperzine A is 0.028%.

[0038] 2) Extraction: Put the crushed raw materials into the cleaned extraction tank, add 1300kg of 40°C, PH3.0 acid water for soaking and extraction, set the extraction time for 5 hours, and stir for 10 minutes every 30 minutes; the first time After the extraction was completed, repeat three times, and all the extracts were combined (because of the test, the fourth extract was not applied).

[0039] 3) Centrifugation: The extract obtained in step (2) was centrifuged with a decanter centrifuge, and then passed through a disc centrifuge to obtain 4758 kg of centrifuge, and the temperature of the feed liquid was 41°C.

[0040] 4) Ultrafiltration: Pass the centrifugate obtained in step (3) through an ultrafiltration membrane of 10,000 to 30,000 Daltons. The pressure of the membrane is controlled at 1.6MPa, and the temperature of the ...

Embodiment 3

[0046] 1) Pretreatment of raw materials: Take 100kg of raw materials that meet the process requirements, and the content of huperzine A is 0.028%.

[0047] 2) Extraction: Put the crushed raw materials into the cleaned extraction tank, add 1500kg of 43°C, PH3.5 acid water for soaking and extraction, set the extraction time for 6 hours, and stir for 10 minutes every 30 minutes; the first time After the extraction was completed, repeat three times, and all the extracts were combined (because of the test, the fourth extract was not applied).

[0048] 3) Centrifugation: The extract obtained in step (2) was centrifuged with a decanter centrifuge, and then passed through a disc centrifuge to obtain 5667 kg of centrifuge, and the temperature of the feed liquid was 44°C.

[0049] 4) Ultrafiltration: pass the centrate obtained in step (3) through an ultrafiltration membrane of 10,000 to 30,000 Daltons, the pressure of the membrane is controlled at 2.0MPa, and the temperature of the mate...

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PUM

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Abstract

The invention provides a huperzine A production method suitable for industrial production and relates to a huperzine A production method. The huperzine A production method comprises the following specific steps of pretreatment of raw materials, extraction, centrifugation, ultra-filtration, nano-filtration, PH value regulation, concentration, microwave drying and smashing. The huperzine A production method adopts a membrane technology for separation and purification. Compared with other purification modes such as macroporous resin adsorption and solvent extraction, the huperzine A production method has the advantages of being safe, environmentally friendly and capable of saving energy, only using a pure water solvent, not adopting an organic solvent and the like, the operation is simple, the product is safe, environmentally friendly, good and inexpensive, and continuous large-scale industrial production can be achieved.

Description

technical field [0001] The invention relates to a production method of huperzine A, in particular to a method suitable for industrial production of high-purity huperzine A. Background technique [0002] Huperzine A is used for middle-aged and elderly people with benign memory impairment and various types of dementia, memory cognitive function and emotional behavior disorders. Can still be used to treat myasthenia gravis. Its Chinese aliases are: Fordine, Haberin, Zhulin Ante. This product is a reversible cholinesterase inhibitor, which has a selective inhibitory effect on true cholinesterase and has high biological activity. [0003] At present, there are more and more diseases such as benign memory impairment and various types of dementia, memory cognitive function and emotional behavior disorders in middle-aged and elderly people, and the demand for this product is also increasing. At present, huperzine A has a good therapeutic effect on this type of disease in the worl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
CPCC07D221/22Y02P20/10Y02P20/50
Inventor 龙伟岸黄华学
Owner JIANGXI HAIFU BIOENG
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