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Method for separating total alkaloids from Melaleuca extract

A technology of total alkaloids and Melaleuca tower, which is applied in the direction of medical preparations containing active ingredients, plant/algae/fungus/moss components, medical raw materials derived from ferns/filamentous plants, etc., and can solve the problem of total alkaloids Low yield and other problems, to achieve the effect of coherent process, large processing capacity and low production cost

Active Publication Date: 2022-04-19
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the step of extracting total flavonoids by ethanol reflux in this method, some total alkaloids will be leached by ethanol, which will inevitably lead to a low yield of subsequent total alkaloids.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Dissolving: get 3 kg of Melaleuca extract, dissolve with 90L ethyl acetate, remove insoluble matter by filtration, and obtain Melaleuca extract ethyl acetate solution;

[0048] (2) Stripping: With 2wt% hydrochloric acid aqueous solution, which contains 0.01wt% tetradecyltrimethylammonium chloride, 0.03wt% alkylphenol polyoxyethylene ether OP-30, stripping the Melaleuca extract Ethyl acetate solution, back extraction twice (the acid water consumption of back extraction for the first time is 150L, ​​and the acid water consumption of back extraction for the second time is 120L), merge acid water layer;

[0049] (3) Decolorization, filtration, concentration: add 0.2kg gac to the acid water layer, stir and decolorize for 2 hours, coarse filter, and then filter with a nanofiltration membrane with a molecular weight cut-off of 500Da (filter pressure 0.3Mpa), the nanofiltration membrane filtrate is at temperature Concentrate under reduced pressure at a temperature of 65°C a...

Embodiment 2

[0055] (1) dissolving: get Melaleuca pagoda extract 3kg, dissolve with 75L dichloromethane, filter and remove insoluble matter, obtain the Melaleuca pagoda extract dichloromethane solution;

[0056] (2) Stripping: use 1.5wt% sulfuric acid aqueous solution, which contains 0.02wt% cetyltrimethylammonium chloride, 0.02wt% alkylphenol polyoxyethylene ether OP-30, back extraction Melaleuca column extraction Thin dichloromethane solution, back extraction twice (the sour water consumption of back extraction for the first time is 150L, ​​and the acid water consumption of back extraction for the second time is 150L), merges acid water layer;

[0057] (3) Decolorization, filtration, and concentration: add 0.3 kg of diatomaceous earth to the acidic water layer, stir for 3 hours to decolorize, coarsely filter, and then filter with a nanofiltration membrane with a molecular weight cut-off of 300Da (filtration pressure 0.5Mpa), and the nanofiltration membrane filtrate Concentrate under redu...

Embodiment 3

[0063] (1) Dissolving: get Melaleuca pagoda extract 3kg, dissolve with 60L chloroform, filter and remove insolubles, get Melaleuca pagoda extract chloroform solution;

[0064] (2) stripping: with 2.5wt% phosphoric acid aqueous solution, wherein containing 0.015wt% tetradecyl trimethylammonium chloride, 0.03wt% fatty acid polyoxyethylene ester A105, stripping the chloroform solution of the Melaleuca tower extract, Back extraction twice (the acid water consumption of back extraction is 180L for the first time, and the acid water consumption of back extraction for the second time is 150L), and the acid water layer is combined;

[0065] (3) Decolorization, filtration, concentration: add 0.3kg activated clay to the acid water layer, stir and decolorize for 3 hours, coarse filter, then use the nanofiltration membrane filtration (filter pressure 0.4Mpa) that the molecular weight cut off is 300Da, the nanofiltration membrane filtrate is in Concentrate under reduced pressure at a tempe...

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Abstract

The present invention relates to a method for separating total alkaloids from Melaleuca extract, comprising the following steps: (1) dissolving; (2) stripping; (3) decolorizing, filtering, and concentrating; (4) extracting; (5) ) silica gel chromatography. In the stripping of step (2), the extract obtained in step (1) is stripped with acidic water containing a surfactant. The present invention optimizes and screens the conditions and operations of each step, and finally uses a comparative The method is simple, and the alkaloids from the Melaleuca tower are prepared with a high yield, and the high-purity 6β-hydroxyhuperzine A, huperzine A and huperzine B are further separated. The method of the invention has small raw material processing capacity, less solvent consumption, less emulsification in the extraction process, short production cycle, coherent and simple process, strong operability, low production cost, safety and environmental protection, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating natural active ingredients from the extract of Melaleuca, in particular to a method for separating total alkaloids from the extract of Melaleuca. Background technique [0002] Melaleuca pagoda is Lycopodium Serratum Thunb., a genus of Lycopodium Serratum in the Lycopodium family. It is a rare and rare wild medicinal plant with the whole herb used as medicine. Folks use the whole herb to treat diseases such as bruises, snake bites, congestion, swelling and pain, and schizophrenia. [0003] Melaleuca is rich in a large number of alkaloids: huperzine A, huperzine B, 6β-hydroxyhuperzine A, lycodine, lycodine, lycodine, lycopine, lycothine, melaleuca Tower base, Melaleuca tanine, Melaleuca tanidine, Melaleuca tanidine, Melaleuca tanidine, lycothrine, lustrous huperzine, N-methylhuperzine B, snake feet Huperzine and more. [0004] Huperzine A, a very important natural plant alkaloid in Melaleuca, is a poten...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/22A61K36/11
CPCA61K36/11A61K2236/33A61K2236/35A61K2236/55A61K2236/51
Inventor 李伟黄华学
Owner HUNAN HUACHENG BIOTECH
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