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Method for extracting huperzine A

A technology for huperzine A and methanol, applied in the field of extracting huperzine A, can solve the problems of high extraction difficulty, low extraction efficiency, improved yield and the like, and achieves simple and easy-to-operate methods, simple and controllable methods, and small solvent consumption. Effect

Pending Publication Date: 2019-08-02
YUNNAN HANDE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) Huperzine A exists in a very low amount in nature, and contains a large amount of impurities. The extraction is complicated, difficult, and low yield; (2) At present, there are many extraction methods for Melaleuca huperzine A, some of which are Although the purity of the extracted product is high, the yield is very low and the production volume is small, so it is impossible to promote industrial production; that is, some extraction methods can improve the yield, but because of high operability requirements, complicated control, and immature technology, etc. Facilitate amplification and industrial production;
[0009] (3) Due to the long production cycle and low extraction efficiency of huperzine A, it is difficult to promote application and large-scale production, and it is difficult to obtain ideal curative effect for synthetic products;
[0010] (4) At present, some extraction processes use acid water extraction, which causes serious environmental pollution and is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: The method for extracting huperzine A is as follows:

[0031] (1) Use 500kg, 20-mesh dried Melaleuca tower as raw material, with huperzine A content of 0.018%, soak the raw material with 1500L formic acid-methanol mixed solution (the volume ratio of formic acid and methanol is 1:500) at 35°C for 8 hours, Filter, then soak the filter residue in 1500L formic acid-methanol mixed solution repeatedly for 6 hours, filter, collect the combined filtrate, and concentrate by rotary evaporation to obtain 31.5kg of Huperzine A crude extract, content 0.27%;

[0032] (2) The crude extract of huperzine A was dissolved in methanol at 55°C, then the pH was adjusted to 6-7 with 20% sodium bicarbonate solution, extracted twice with chloroform, the chloroform layer was collected, concentrated and dried to obtain stone The crude product of phenine A, the content is 2.53%;

[0033] (3) The crude product of huperzine A is dissolved in chloroform, and after it is dissolved, a de...

Embodiment 2

[0037] Embodiment 2: the method for extracting huperzine A is as follows:

[0038] (1) Use 500kg, 10-mesh dried Melaleuca tower as raw material, with huperzine A content of 0.018%, soak the raw material in 2000L formic acid-methanol mixed solution (the volume ratio of formic acid and methanol is 1:600) at 35°C for 8 hours, Filter, then soak the filter residue in 1500L formic acid-methanol mixed solution repeatedly for 6 hours, filter, collect the combined filtrate, and concentrate by rotary evaporation to obtain huperzine A crude extract 32.4kg; content 0.26%;

[0039] (2) The crude extract of huperzine A was dissolved in methanol at 60°C, then the pH was adjusted to 6-7 with 25% sodium bicarbonate solution, extracted with chloroform three times, the chloroform layer was collected, concentrated and dried to obtain stone Pine A crude product; content 2.61%;

[0040] (3) The crude product of huperzine A is dissolved in chloroform, and after it is dissolved, a decolorizing agent...

Embodiment 3

[0044] Embodiment 3: The method for extracting huperzine A is as follows:

[0045] (1) Use 500kg, 10-20 mesh dry Melaleuca tower as raw material, soak the raw material with 1700L formic acid-ethanol mixed solution (the volume ratio of formic acid and ethanol is 1:450) at 45°C for 8 hours, filter, and use 1500L of filter residue The formic acid-methanol mixed solution was repeatedly soaked for 7 hours, filtered, collected and combined filtrate, and concentrated by rotary evaporation to obtain 32.1 kg of crude extract of huperzine A, with a content of 0.25%;

[0046] (2) Dissolve the crude extract of Huperzine A in methanol at 65°C, then adjust the pH to 6-7 with 10% sodium carbonate solution, extract twice with dichloromethane, collect the dichloromethane layer, concentrate and dry Huperzine A crude product was obtained, with a content of 2.58%;

[0047] (3) Dissolve the crude product of huperzine A in chloroform, after it dissolves, add a decolorizing agent (prepared by mixin...

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PUM

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Abstract

The invention discloses a method for extracting huperzine A. The method comprises the following steps: soaking huperzia serrata with an acidic organic solvent to extract total huperzine, adjusting pHvalue after concentration, and then carrying out extraction, decoloration and mud flocculation, recrystallization, normal phase column chromatography and recrystallization to obtain huperzine A. The method is simple and easy in operation, little in pollution, short in production cycle, low in cost and high in yield, and is applicable to industrial application and market popularization.

Description

technical field [0001] The invention relates to an industrialized production method for extracting huperzine A from a dried melaleuca tower. Background technique [0002] Melaleuca ( Huperzia serrata Trev.) is also known as Huperus serrata and Huperus serrata. It is the whole herb of the perennial herb Huperus serrata in the family Huperzaceae. It is one of the endemic plants in my country. It is widely distributed all over the country. It can be used as medicine, and is commonly used in the folk to treat bruises, internal injuries, bleeding, bruises, swelling and pain, snake bites, etc. [0003] Huperzine A is a natural alkaloid isolated from Huperzia serrata (melaleuca), which has the basic properties of alkaloids. It is easily soluble in chloroform, soluble in methanol, ethanol, slightly soluble in water. The molecular weight of huperzine A is 242.32, and the molecular formula is C 15 h 18 N 2 O. [0004] Huperzine A has a significant effect on the treatment of ear...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
CPCC07D221/22
Inventor 马回民杨青春胡倩赵泽熙
Owner YUNNAN HANDE BIO TECH
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