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Preparation method and system for high-purity huperzine a liquid phase

A technology of huperzine A solution and huperzine A, which is applied in the field of alkaloid extraction, can solve the problems of limited application range, low stability, complicated operation, etc., and achieves wide application range, low production cost, Simple operation effect

Pending Publication Date: 2017-05-31
湖南铭沃生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main problem to be solved by this application is to provide a liquid-phase preparation method of high-purity huperzine A with simple operation, good stability, high yield, high purity, and low energy consumption, so as to solve the problem of complex operation and limited scope of application of a preparation method. , low stability, low yield, low purity and high energy consumption

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  • Preparation method and system for high-purity huperzine a liquid phase

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Embodiment 1

[0047] Such as figure 1 As shown in the schematic flow sheet of the liquid-phase preparation method of high-purity huperzine A provided by the present invention, a liquid-phase preparation method of high-purity huperzine A is characterized in that, comprising:

[0048] Step 1 1: Take the crude extract of Melaleuca Tower, dissolve it in aqueous methanol solution, and separate by filtration to obtain insoluble matter and filtrate;

[0049] Step 2 2: The filtrate described in Step 1 1 is subjected to high-pressure liquid phase preparation, and the huperzine A fraction is collected;

[0050] Step 3 3: performing liquid phase analysis on the fraction described in step 2 2 to obtain a fraction that meets the purity requirements;

[0051] Step 4 4: Combine the fractions obtained in Step 3 3 and concentrate under reduced pressure to obtain the crude product of huperzine A.

[0052] Further, it also includes:

[0053] Step 5 5: Freeze-dry the crude huperzine A product described in s...

Embodiment 2

[0066] The instrumentation involved in the present embodiment and detection condition are as follows:

[0067] High performance liquid chromatography: UV detection wavelength is 310nm, flow rate is 1mL / min, mobile phase is methanol and pure water, the ratio is 60:40; semi-preparative high performance liquid chromatography: UV detection wavelength is 310nm, flow rate is 4mL / min , mobile phase is methanol and pure water, its ratio is 60:40;

[0068] The parameters of the chromatographic column for analysis are 5 μm, 120A, 4.6mm*250mm; the parameters of the chromatographic column for preparation are 10 μm, 120A, 10mm*250mm.

[0069] The concrete steps of high-purity huperzine A liquid phase preparation method are:

[0070] Dissolution: Weigh 0.5g of Melaleuca crude extract (about 5% of huperzine A content), add 2ml of 50% methanol aqueous solution, ultrasonically dissolve for 10min, filter with 0.45μm organic filter membrane, and filter the remaining filter residue Wash and fil...

Embodiment 3

[0076] The instrumentation involved in the present embodiment and detection condition are as follows:

[0077] Liquid chromatography: UV detection wavelength is 310nm, flow rate is 1mL / min, mobile phase is methanol and pure water, the ratio is 60:40; LC6000 preparative high performance liquid chromatography: UV detection wavelength is 310nm, flow rate is 80mL / min , mobile phase is methanol and pure water, its ratio is 60:40;

[0078] The parameters of the chromatographic column for analysis are 5μm, 120A, 4.6mm*250mm; the parameters of the chromatographic column for preparation are 50mm dynamic axial compression preparative column system, and the parameters of chromatographic packing are 10μm, 120A;

[0079] Dissolution: Weigh 50g of Melaleuca crude extract (about 5% huperzine A content), add 200ml 50% methanol aqueous solution, ultrasonically dissolve for 10min, filter with 0.45μm organic filter membrane, and use the remaining filter residue after filtration 50ml of 50% meth...

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Abstract

The invention provides a preparation method for a high-purity huperzine a liquid phase. The method is characterized by comprising the steps that 1, a lycopodium serratum crude extractive is taken and placed into a methyl alcohol water solution to be dissolved, and filtering separation is performed to obtain undissolved substances and a filtrate; 2, the filtrate obtained in the step 1 is subjected to high pressure liquid phase preparation, and huperzine a fractions are collected; 3, the fractions obtained in the step 2 are subjected to liquid phase analysis to obtain fractions meeting the purity requirement; 4, the fractions obtained in the step 3 are combined, and vacuum concentration is performed to obtain a huperzine a crude product. Equipment is simple, operation is simple, the production steps are simple, auxiliary raw materials are easy to obtain, and the production cost is low; the production process is high in stability, and reappearing is likely to be achieved; the product yield is high, the raw material utilization rate is high, the auxiliary raw materials can be repeatedly utilized, the production cost is reduced, and environmental protection is achieved; the produced product is high in purity, so that the application range is wide, and the requirement for medical purposes and medicinal purposes can be met; the production cost is low in energy consumption, and the method saves energy and is environmentally friendly and scientific.

Description

technical field [0001] The invention relates to an extraction method of alkaloids, in particular to a method and system for extracting and separating huperzine A from a Melaleuca tower. Background technique [0002] The Melaleuca Pagoda is a fern of the genus Huperzia in the family Huperzaceae, also known as Huperzia serrata and King of Help. It is mainly distributed in the Northeast, the Yangtze River Basin and Fujian, Guangdong, Guangxi, Yunnan, Guizhou and other provinces. Folks often use the whole herb as medicine, which is poisonous and used for reducing fever, hemostasis, reducing swelling and detoxification, and traumatic injuries. The alkaloids contained in Melaleuca are of high value, especially huperzine A, which is a reversible cholinesterase inhibitor, which has a selective inhibitory effect on true cholinesterase, and its biological activity High, after entering the central nervous system, it is more distributed in the frontal lobe, temporal lobe, hippocampus ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
CPCC07D221/22
Inventor 赵志远曾昭明
Owner 湖南铭沃生物科技股份有限公司