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Separation and purification method of rhodojaponin-III monomer

A technology for the separation and purification of the toxin and its separation and purification, which is applied in the field of separation and purification of the active ingredients of traditional Chinese medicine, which can solve the problems of long production cycle and low yield, and achieve the effect of short production cycle, high yield and strong target

Active Publication Date: 2013-04-03
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] According to related searches, at present, for the separation of aminotoxin Ⅲ monomer, the method of repeated crystallization after silica gel column chromatography is mainly used, which has a long production cycle and low yield

Method used

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  • Separation and purification method of rhodojaponin-III monomer
  • Separation and purification method of rhodojaponin-III monomer
  • Separation and purification method of rhodojaponin-III monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A method for separating and purifying the aminotoxin III monomer, comprising the following process steps:

[0042] A extraction

[0043] Grind 100Kg of the dry herbal medicine Azalea into a coarse powder of 1-4mm, and put it into a volume of 2x10 33 In the extraction tank of L, add 600L of methanol solution with a concentration of 90% by mass, extract 3 times at 60°C for 3 hours each time, filter the extract, combine the filtrates, concentrate at 60°C to recover methanol, and obtain a concentrated solution with a relative density of 1.1 The paste is about 80L to be processed in the next step;

[0044] B Extraction of total toxins

[0045] Dilute the concentrated extract obtained in step A with water to a relative density of 0.85g / mL (measured at about 60°C) to obtain a total of 100L of solution, add an equal volume of ethyl acetate to extract 4 times, and transfer the merinotoxin III to acetic acid In the ethyl ester solution, the upper layer solution was separated, ...

Embodiment 2

[0055] A method for separating and purifying the aminotoxin III monomer, comprising the following process steps:

[0056] A extraction

[0057] Grind 300Kg of the dried herbal medicine Azalea chinensis into 1-4mm coarse powder, and put it into a volume of 4x10 33 In the extraction tank of L, add the methanol solution 2.4x10 that mass percent concentration is 85% 3 L, extracted 4 times at 80°C, each time for 1.5 hours, filtered the extract, combined the filtrate, concentrated at 85°C to recover methanol, and obtained about 180L of concentrated extract with a relative density of 1.0 to be processed in the next step;

[0058] B. Extraction of total toxins

[0059] Dilute the concentrated extract obtained in step A with water to a relative density of 0.9g / mL (measured at about 60°C), and a total of about 200L of solution is obtained, and an equal volume of ethyl acetate is added to extract 5 times, so that the toxin III is transferred to In the ethyl acetate solution, the upper...

Embodiment 3

[0069] A method for separating and purifying the aminotoxin III monomer, comprising the following process steps:

[0070] A extraction

[0071] Grind 50Kg of the dried herbal medicine Azalea chinensis into 1~4mm coarse powder, and put it into a volume of 1x10 33 Add 500L of ethanol solution with a mass percentage concentration of 70% to an extraction tank of L, extract 3 times at 100°C for 1 hour each time, filter the extract, combine the filtrate, concentrate at 90°C to recover ethanol, and obtain a concentrated immersion solution with a relative density of 1.1 The paste is about 20L to be processed in the next step;

[0072] B Extraction of total toxins

[0073] Dilute the concentrated extract obtained in step A with water to a relative density of 0.7g / mL (measured at about 60°C) to obtain a total of 28L of solution, add an equal volume of ethyl acetate to extract 3 times, and transfer the toxin III to acetic acid In the ethyl ester solution, the upper layer solution was ...

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Abstract

The invention provides a separation and purification method of a rhodojaponin-III monomer, and belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines. The separation and purification method comprises the following steps in sequence: based on ericaceous plant rhododendron molle as a raw material, carrying out alcohol extraction, ethyl acetate extraction and preparative high performance liquid chromatography separation; and concentrating and drying to obtain the rhodojaponin-III monomer. According to the preparation method, the optimal technology and parameter conditions are utilized, thus the content of the rhodojaponin-III in the product is up to more than 98%; and the method is simple and convenient for operation in the whole technological process, stable in technology, low in cost, suitable for mass production, high in separation efficiency and high in purity of product, and can realize high-purity separation and preparation of the rhodojaponin-III monomers as mass.

Description

technical field [0001] The invention relates to a preparation method of a plant compound monomer, in particular to a method for extracting and isolating the aminotoxin III monomer from roe deer, and belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines. Background technique [0002] Rhodojaponin Ⅲ is also called rhodojaponin Ⅲ, Rhodojaponin Ⅲ, molecular formula is C 20 h 32 o 6 , the molecular weight is 368, and the structural formula is as follows: [0003] [0004] Pyrethrin III is derived from Rhododendron molle G. Don, a plant of the Rhododendaceae family. There are two main mechanisms, one is to act on the nervous system, affecting the activity of adenosine triphosphate (ATP) enzyme in nerve cells, blocking nerve conduction, and affecting the opening of ion channels; the other is to destroy the midgut biofilm system, affecting the digestive tract enzyme system and detoxifying plum system activity. Th...

Claims

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Application Information

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IPC IPC(8): C07D303/14C07D301/32
Inventor 文焕松夏柯姚志容李启发郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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