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Method for refining stachydrine from motherwort

A technology of motherwort and stachydine, applied in the direction of organic chemistry and the like, can solve the problems of high energy consumption, low total alkaloid yield, low content of stachydine hydrochloride, etc., and achieves low energy consumption, less impurities, and reduced dosage. Effect

Inactive Publication Date: 2010-10-20
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above method gained stachydrine content is low, and total alkaloid yield is low, and energy consumption is big

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 5kg of motherwort, crush it, add 50L of 3% hydrochloric acid solution, extract dynamically for 3 hours, extract twice or twice, combine the extracts and filter, add 2L of strong acid cation 732 resin column for adsorption, wash with deionized water and neutralize, 12L of 15% sodium chloride Solution elutes stahydrine, collects fractions, adds molecular weight cut-off 3000 hollow cellulose membrane for ultrafiltration, collects permeate, concentrates under reduced pressure to 200ml, adds ammonia water and stirs to pH12, takes n-butanol 600ml and mixes and extracts, extracts 3 times, Collect the extract and add 18g of activated carbon to reflux for decolorization, filter and concentrate to 200ml, add 6ml of diethyl ether to place crystallization, filter out the crude crystals, reflux with absolute ethanol to dissolve and filter, add 5ml of diethyl ether, freeze crystallization 3 times, filter out and dry to obtain water Threonine 13g, content 95%.

Embodiment 2

[0027] Take 5kg of motherwort, crush it, add 50L of 5% hydrochloric acid solution, extract dynamically for 2 hours, extract twice or twice, combine the extracts and filter, add 2L of strong acid cation 732 resin column for adsorption, wash with deionized water and neutralize, 10L of 20% sodium chloride The solution elutes stahydrine, collects fractions, adds molecular weight cut-off 3000 hollow cellulose membrane for ultrafiltration, collects the permeate, concentrates under reduced pressure to 200ml, adds ammonia water and stirs to pH10, takes 800ml of n-butanol and extracts, extracts twice, Collect the extract and add 20g of activated carbon to reflux for decolorization, filter and concentrate to 300ml, add 15ml of diethyl ether and place it for crystallization, filter out the crude crystals, reflux with absolute ethanol to dissolve and filter, add 10ml of diethyl ether, freeze crystallization twice, filter out and dry to obtain water Threonine 12g, content 94%.

Embodiment 3

[0029] Take 5kg of motherwort, crush it, add 30L of 3% hydrochloric acid solution, extract dynamically for 3 hours, extract two or three times, combine the extracts and filter, add 2L of strong acid cation 732 resin column for adsorption, wash with deionized water and neutralize, 12L of 10% sodium chloride The solution elutes stahydrine, collects fractions, adds molecular weight cut-off 3000 hollow cellulose membrane for ultrafiltration, collects the permeate, concentrates under reduced pressure to 300ml, adds ammonia water and stirs until pH12, takes 600ml of n-butanol and mixes and extracts, extracting 3 times, Collect the extract and add 30g of activated carbon to reflux for decolorization, filter and concentrate to 300ml, add 10ml of diethyl ether and place it for crystallization, filter out the crude crystals, reflux with absolute ethanol to dissolve and filter, add 10ml of diethyl ether, freeze and crystallize 3 times, filter out and dry to obtain water Threonine 10g, con...

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Abstract

The invention relates to a method for refining stachydrine from motherwort. The processing steps are as follows: aqueous hydrochloric acid solution extraction under the normal temperature, strong-acid cation resin adsorption, 10 to 20 percent of saline solution elution, hyperfiltration membrane hyperfiltration, ammonification, n-butyl alcohol extraction, crystallization and ethanol aether solution recrystallization. When the method is adopted to produce the stachydrine, pollution is little, energy consumption is low, and the product yield is high.

Description

Technical field: [0001] The invention relates to a method for extracting and purifying stachydrine from motherwort leaves, in particular to a process for extracting and purifying stachydrine with acid water and membrane. Background technique: [0002] Motherwort Leonurus japonicus Houtt. The fresh or dry aerial part of Lamiaceae plant Leonurus japonicus Houtt. Slightly cold in nature, bitter and pungent in taste, it can remove blood stasis and generate new energy, promote blood circulation and regulate menstruation, diuresis and reduce swelling. It is an important medicine used by doctors of all ages to treat gynecological diseases. Modern medical research has proved that Motherwort contains Leonurine, stachydrine, rutin, fumaric acid, Leonurine A and Leonurine B, stachyose, phytosterols, resins, fatty oils, lauric acid, linoleic acid, β-linoleic acid and oleic acid. [0003] According to modern clinical and animal practice, motherwort extract and decoction have a strong a...

Claims

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Application Information

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IPC IPC(8): C07D207/16
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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