Method for separating and purifying huperzine by molecular imprinting technology

A technology for huperzine A and molecular imprinting, which is applied in the field of separation and purification of huperzine A by molecular imprinting technology, can solve the problems of complex process, large amount of organic solvent, expensive equipment, etc., and achieves increased extraction yield, shortened extraction time, The effect of high product yield

Inactive Publication Date: 2012-06-13
杭州华东医药集团康润制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Above-mentioned various methods, although Chinese patent CN101134743A, Chinese patent CN101602727A, Chinese patent CN10880259A, although the isolated huperzine A has higher purity, the process is complex, the amount of organic solvent is large, time-consuming, and high in cost, and is not suitable for industrial production; Chinese patent The purity of huperzine A isolated by CN101747275A is relatively low; Chinese patent CN1448390A, Chinese patent CN1587260A, and Chinese patent CN101693689A adopt high-performance liquid chromatography and high-speed countercurrent chromatography to separate huperzine A respectively, and obtain product purity higher, but production capacity Small, expensive equipment, mostly limited to laboratory applications

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1, a kind of method for separating and purifying huperzine A by molecular imprinting technology, carries out the following steps successively:

[0037] 1) Preparation of molecularly imprinted polymer of huperzine A

[0038] Measure the chloroform of 10ml in the 25ml test tube, be 98% Huperzine A (template molecule) with 0.60g mass content, 12.05g ethylene glycol dimethacrylate (crosslinking agent), 10.06g methacrylic acid ( Functional monomer), 0.03g of azobisisobutyronitrile (initiator) were sequentially added into the above-mentioned test tube, sealed, and dissolved by ultrasonic (40KHz frequency) for 20min. The homogeneously mixed polymerization solution was filled with nitrogen for 10 min. Put the test tube in a water bath at 65°C, heat and polymerize for 4 hours, then raise the temperature to 68°C after polymerization, and continue heating for 2 hours to complete the polymerization.

[0039]The obtained bulk polymer is taken out, ground to pass 400 mes...

Embodiment 2

[0047] Embodiment 2, a method for separating and purifying huperzine A by molecular imprinting technology, the following steps are carried out successively:

[0048] 1) Preparation of molecularly imprinted polymer of huperzine A:

[0049] Measure the acetone of 30ml in the 100ml flask, be 98% huperzine A with 1.0g mass content, 21.0g pentaerythritol triacrylate, 14.56g 4-vinylphenylboronic acid (also known as: 4-vinylphenylboronic acid), 0.05 g of azobisisobutyronitrile was sequentially added into the flask, sealed, and dissolved by ultrasonic (40KHz frequency ultrasonic) for 30 min. The homogeneously mixed polymerization solution was filled with nitrogen, and heated in a water bath at 65°C for 12 hours to complete the polymerization.

[0050] The obtained bulk polymer is taken out, ground to pass 200 mesh, sieved in water with a 200 mesh stainless steel sieve by wet method, suction filtered, and the obtained particle size is less than 200 mesh. Ethanol extracts the residual...

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Abstract

The invention discloses a method for separating and purifying huperzine by a molecular imprinting technology, which includes the following steps: 1 huperzia serrata is smashed and extracted in ultrasonic counter-current mode, obtained extracting solution is decompressed and concentrated, and then active carbon is added in the extracting solution to perform decoloration; 2 the decolorized extracting solution is arranged on a solid phase column, huperzine molecular imprinting polymer serving as a solid phase is installed in the solid phase column, 5% to 10% of ethanol water or methanol water is used for elution, 40% to 50% of ethanol water or methanol water is used for elution till eluent is colorless, an disassembling column enables the solid phase to be taken out from the solid phase column, and 60% to 70% of ethanol water or methanol water is used for extracting adsorbed huperzine monomers in the solid phase to obtain extraction liquid; and 3 the extraction liquid is decompressed, concentrated and recrystallized by using solvent to obtain the huperzine. The method for preparing the huperzine has the advantages of being safe, easy and simple to operate, low in cost, short in production cycle, high in purity and the like.

Description

technical field [0001] The invention relates to a method for separating and purifying huperzine A by molecular imprinting technology. Background technique [0002] Huperzine A (Hup A for short), also known as fordine, is a natural alkaloid isolated from Huperzine genus Serpentine (melaleuca), which is a powerful reversible alkaloid. Acetylcholinesterase (AChE) inhibitors have significant curative effects on the treatment of Alzheimer's disease, simple memory impairment and myasthenia gravis, and the drug effect lasts for a long time without serious adverse reactions. It is currently the most effective treatment for the above diseases at home and abroad. Drugs are of great concern. Due to its high therapeutic index and long duration of action, it has been listed as one of the second-generation cholinesterase inhibitors internationally. However, Hup A exists in a very low amount in nature and contains a large amount of impurities, making it difficult to separate and purify. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
Inventor 蒋风沈生荣周建仁王维边锋
Owner 杭州华东医药集团康润制药有限公司
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