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A method for separating and preparing iridoids from Duyiwei

A unique technology of iridoids, applied in the field of plant purification, can solve the problems of unsuitability for industrial production, complex process route, difficult operation, etc., and achieve strong controllability of product quality, simple process route, and low production cost Effect

Active Publication Date: 2020-07-17
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the disadvantages of complex process route, large melting consumption, long cycle, low yield, high cost, difficult operation and unsuitability for industrial production in the prior art, and to provide a method for separating and preparing The iridoid method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A method for separating and preparing iridoids from Duyiwei, comprising the following steps:

[0041] Step 1) raw material pretreatment

[0042] Crush 100kg of raw materials alone, pass through a 60-mesh sieve, and use subcritical extraction to collect the extraction residue;

[0043] Step 2) Extract

[0044] Wet the extraction residue with water of equal mass, and after standing for 30 to 60 minutes, use ethyl acetate 5 times the mass of the raw material to extract at 60°C for 3 times, each time for 1.5 hours, filter, collect the filtrate and concentrate the filtrate to About 100kg;

[0045] Step 3) alkaline water extraction

[0046] The concentrated filtrate in step 2) was extracted at least twice with an equal volume of aqueous ammonia having a mass concentration of 3%, and the aqueous ammonia layers were combined;

[0047] Step 4) gradient extraction, crystallization

[0048] In the combined ammonia water layer, add a mass concentration of 1% hydrochloric acid ...

Embodiment 2

[0053] A method for separating and preparing iridoids from Duyiwei, comprising the following steps:

[0054] Step 1) raw material pretreatment

[0055] Crush 100kg of raw materials alone, pass through a 100-mesh sieve, and use subcritical extraction to collect the extraction residue;

[0056] Step 2) Extract

[0057] Wet the extraction residue with water of equal mass, and after standing for 30-60 minutes, use n-butanol 10 times the mass of the raw material to extract at 80°C for 3 times, each time for 1.5 hours, filter, collect the filtrate and concentrate the filtrate to About 300kg;

[0058] Step 3) alkaline water extraction

[0059] The filtrate concentrated in step 2) was extracted at least twice with an equal volume of 3% sodium bicarbonate solution, and the alkaline water layers were combined;

[0060] Step 4) gradient extraction, crystallization

[0061] In the combined alkaline water layer, add a citric acid solution with a mass concentration of 3% to adjust the pH...

Embodiment 3

[0066] A method for separating and preparing iridoids from Duyiwei, comprising the following steps:

[0067] Step 1) raw material pretreatment

[0068] Crush 100kg of raw materials alone, pass through an 80-mesh sieve, and use subcritical extraction to collect the extraction residue;

[0069] Step 2) Extract

[0070] Wet the extraction residue with water of equal mass, and after standing for 30 to 60 minutes, use ethyl acetate 10 times the mass of the raw material to extract at 80°C for 3 times, each time for 1.5 hours, filter, collect the filtrate and concentrate the filtrate to About 200kg;

[0071] Step 3) alkaline water extraction

[0072] The filtrate concentrated in step 2) was extracted at least twice with an equal volume of ammonia water having a mass concentration of 2%, and the ammonia water layer was combined;

[0073] Step 4) gradient extraction, crystallization

[0074] In the combined ammonia water layer, add a mass concentration of 1% sulfuric acid solution...

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PUM

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Abstract

The invention provides a method for separation preparation of an iridoid compound from Lamiophlomis rotata. The method of the present invention eliminates conventional column separation and other complex processes, and comprises: crushing a raw material, screening, carrying out subcritical extraction pretreatment, extracting the residue obtained after subcritical extraction by using ethyl acetateor n-butanol to remove most of flavonoid glycosides, phenethanol glycosides and other high-polarity impurities, further extracting with ammonia water or a sodium bicarbonate solution, transferring shanzhiside methyl ester and 8-O-acetyl shanzhiside methyl ester to an alkaline water layer, and carrying out gradient extraction with different mass ratios of chloroform-methanol mixed solutions to successfully separate the shanzhiside methyl ester and the 8-O-acetyl shanzhiside methyl ester. According to the present invention, the method can avoid the problems of long period, high dissolving consumption, high cost, difficult operation and the like caused by the multiple use of the column separation in the prior art, is suitable for industrial production, and can substantially save the production time.

Description

technical field [0001] The invention belongs to a plant purification method, and in particular relates to a method for separating and preparing iridoids from solitary. Background technique [0002] Duyiwei is a plant of the genus Duyiwei in the family Lamiaceae. It is mainly distributed in Qinghai, Gansu, Sichuan and other provinces of China. It is a commonly used herbal medicine in folk traditions such as Tibetans and Mongolians. Duyiwei mainly contains iridoid glycosides, phenylethanol glycosides and flavonoid glycosides, among which shanzhiside methyl ester and 8-O-acetyl shanzhiside methyl ester are the representative components of its iridoids. Very good hemostasis, procoagulant effect. [0003] Chinese patent document CN101485671B relates to a preparation method of 8-O-acetylshanzhiside methyl ester. In this method, the unique raw material is extracted with ethanol, separated by a polyamide column, and the water eluent is purified by a macroporous adsorption resin, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/04C07H1/06
CPCC07H1/06C07H17/04
Inventor 张瑜王晓莹肖金霞肖红郭伟妮
Owner SHAANXI JIAHE PHYTOCHEM