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Method for extracting and separating huperzine A from huperizia serrata

A technology for Huperzine A and Huperzine serrata, applied in the field of extraction and separation of Huperzine A, can solve the problems of high price of raw materials of Huperzine A, difficult plant source of Huperzine serrata, long growth cycle and the like, and achieves enhanced The effect of market competitiveness, simplified operation and loss reduction

Inactive Publication Date: 2010-06-30
ENSHI QINGJIANG BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although since 1985, a variety of methods for chemically synthesizing huperzine A have been proposed at home and abroad, but due to its complex structure, the cost of its chemical synthesis is much higher than that of plant extraction. Among the plants of the family, the content and reserves of Huperzine A in Huperzia serrata are relatively large
However, the content of huperzine A in Huperzia serrata is only a few ten thousandths, and the source of Huperzine serrata plants is difficult and the growth cycle is as long as 8-10 years, which makes the raw material medicine of huperzine A expensive.

Method used

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  • Method for extracting and separating huperzine A from huperizia serrata
  • Method for extracting and separating huperzine A from huperizia serrata
  • Method for extracting and separating huperzine A from huperizia serrata

Examples

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Effect test

Embodiment 1

[0027] Take 50 g of Huperzia serrata with a crushed mesh of 20 meshes, and extract 4 times with 375 mL of 2% acetic acid solution under stirring at room temperature for 2 hours. The three or four times the extraction liquid is used as the circulating extraction solvent, and the pH of the extraction liquid is adjusted to 9 with ammonia water, and then filtered.

[0028] The SP825 macroporous adsorption resin column was wet-packed in a glass column. After pretreatment according to the method provided by the manufacturer, the pH 9.0 extract was loaded onto the column at a speed of 6BV / h, and the end of the sample loading was monitored by TLC. After saturation, 90% methanol was used as the eluent, and the flow rate was 6 BV / h. Collect the eluate containing the part of Huperzine A, quickly concentrate in vacuum, and dry to obtain crude Huperzine A I.

[0029] 200~300 mesh basic alumina is wet-packed in a 40*300 stainless steel chromatography column with mobile phase, 3390 mg of Huperzi...

Embodiment 2

[0032] Weigh 8Kg of the raw material powder into a 100-liter multifunctional extractor, add 60 liters of 2% acetic acid, stir and extract at room temperature for 2 hours, filter, extract 4 times, and combine the 4 extracts to obtain a total volume of 231 liters of the extract. Adjust the pH of the extract to 9.0 with ammonia and filter.

[0033] The SP825 macroporous adsorption resin column was wet-packed in a glass column. After pretreatment according to the method provided by the manufacturer, the pH 9.0 extract was loaded onto the column at a speed of 6BV / h, and the end of the sample loading was monitored by TLC. After saturation, 90% methanol was used as the eluent, and the flow rate was 6 BV / h. Collect the eluate containing the part of Huperzine A, quickly concentrate in vacuum, and dry to obtain crude Huperzine A I.

[0034] 200~300 mesh basic alumina was packed in 110*1200 stainless steel chromatography column by mobile phase wet method, 103 grams of Huperzine A crude I was...

Embodiment 3

[0037] Weigh 200Kg of raw material powder into a 2000 liter extraction tank, add 1500 liters of 2% acetic acid, stir and extract at room temperature for 2 hours, filter, extract 4 times, and combine the 4 extraction solutions. Adjust the pH of the extract to 9.0 with ammonia.

[0038] The SP825 macroporous adsorption resin column is wet-packed in a stainless steel resin column. After pretreatment according to the method provided by the manufacturer, the pH9.0 extract is loaded onto the column at a speed of 6BV / h, and the end point of the sample loading is monitored by TLC. After saturation, 90% methanol was used as the eluent, and the flow rate was 6 BV / h. Collect the eluate containing the part of Huperzine A, quickly concentrate in vacuum, and dry to obtain crude Huperzine A I.

[0039] 200~300 mesh basic alumina is packed in 110*1200 stainless steel chromatography column by mobile phase wet method, Huperzine A crude product I is divided into several times for basic alumina colum...

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Abstract

The invention relates to a method for extracting and separating huperzine A from huperizia serrata. Aiming at the disadvantages of the existing method of lower yield, higher cost and weak market competitive power, the invention establishes the method for extracting and separating the huperzine A from the huperizia serrata, which comprises the following steps: grinding raw materials, extracting by 2% acetic acid, separating by SP825 micro-pore adsorption resin, column chromatographic separating by alumina B, preparative chromatography purifying by nitrile-group bonding silica gel, concentrating and drying, so as to obtain a finished product. The invention has the benefit that as the new extraction process is adopted, by simplifying operation, reducing loss, improving yield and lowering cost, the market competitive power of the product can be enhanced.

Description

Technical field [0001] The invention relates to a method for extracting and separating Huperzine A from Huperzia serrata. Background technique [0002] Huperzia serrata (Huperzia serrata) is a fern plant of the Huperzia family Huperzia genus, also known as Melaleuca. There are 5 genera and 26 species of Huperzia. In addition to Huperzia serrata in my country, there are also horsetail cedar, Huperzia longipes, Huperzia intermedia, Huperzia Changbaishan, Huperzia Sichuan, Huperzia chinensis, Huperzia chinensis , Guangdong horsetail fir, horsetail fir, narrow-leaf horsetail fir, Longyan horsetail fir, dwarf horsetail fir and other 13 species. According to relevant analysis, the above-mentioned plants in my country basically contain Huperzine A, and they are all medicine resources of Huperzine A. The content of Huperzine A in plants ranges from 0.0003% to 0.006%, and the content and reserves of Huperzia serrata are relatively large. [0003] Huperzia serrata is the most commonly used...

Claims

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Application Information

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IPC IPC(8): C07D221/22B01J20/26B01D15/08
Inventor 向极钎王发松杨永康龙澜李红英
Owner ENSHI QINGJIANG BIO ENG
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