Method of utilizing supercritical CO2 extraction and macroporous resin adsorption separation to extract reserpine from rauvolfia verticillate

A technology of macroporous resin and reserpine, which is applied in the field of extraction and separation of reserpine in Rauwolfia, can solve the problems that are not conducive to industrial production, complicated process steps, high cost of adsorbent, etc., to shorten the production cycle and process The effect of simple process and low cost

Inactive Publication Date: 2015-04-15
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN 101491560 A discloses a method for separating important total alkaloids, but does not involve the process of separating and purifying reserpine; Separation and purification of reserpine by exchange resin adsorption separation, C18 reverse-phase column purification, and crystallization, the process is complex and has many steps, the product yield is low, and the cost of the adsorbent is high, which is not conducive to industrial production; patent CN 101475570 A discloses an ice A method of separation and purification of reserpine by percolation extraction with acetic acid methanol solution, extraction with chloroform for the extract, and recrystallization. Too many toxic reagents are used in the process, and the solvent is easy to remain, which affects product quality.

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  • Method of utilizing supercritical CO2 extraction and macroporous resin adsorption separation to extract reserpine from rauvolfia verticillate

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Experimental program
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Effect test

Embodiment 1

[0026] Preparation of reserpine extract: crush 200g of Rauwolfia root bark, pass through a 10-mesh sieve, put the root powder in a supercritical extraction kettle for supercritical extraction, the temperature of the extraction kettle is 60°C, the pressure of the extraction kettle is 35 MPa, and the separation kettle The temperature of I is 45°C, the pressure of separation kettle I is 8 MPa, the temperature of separation kettle II is 35°C, the pressure of separation kettle II is 5 MPa, 40ml of 95% ethanol is added as entrainer, and the extraction time is 2h;

[0027] After combining the extracts obtained from the separation tank I and the separation tank II, dissolve them with 10% acetic acid (v / v) 50ml, filter and put on the HP-20 resin column, wash the 3 beds with water until neutral, and then use 3 The bed volume was eluted with 15% ethanol (v / v) and 4 bed volumes with 50% ethanol (v / v), and the 50% ethanol (v / v) eluate was collected and concentrated to dryness under reduced ...

Embodiment 2

[0031] Preparation of reserpine extract: crush 200g of Rauwolfia root bark, pass through a 10-mesh sieve, put the root powder in a supercritical extraction kettle for supercritical extraction, the temperature of the extraction kettle is 60°C, the pressure of the extraction kettle is 35 MPa, and the separation kettle The temperature of I is 45°C, the pressure of separation kettle I is 8 MPa, the temperature of separation kettle II is 35°C, the pressure of separation kettle II is 5 MPa, 40ml of 95% ethanol is added as entrainer, and the extraction time is 2h;

[0032] After combining the extracts obtained from the separation tank I and the separation tank II, dissolve them with 10% acetic acid (v / v), filter and put on the AB-8 resin column, wash 3 beds with water until neutral, and then use 3 beds Layer volume of 20% ethanol (v / v) and 5 bed volumes of 60% ethanol (v / v) were eluted, and the 60% ethanol (v / v) eluate was collected and concentrated to dryness under reduced pressure; ...

Embodiment 3

[0036] Preparation of reserpine extract: crush 200g of Rauwolfia root bark, pass through a 10-mesh sieve, put the root powder in a supercritical extraction kettle for supercritical extraction, the temperature of the extraction kettle is 60°C, the pressure of the extraction kettle is 30 MPa, and the separation kettle I temperature is 45°C, separation kettle I pressure is 10 MPa, separation kettle II temperature is 35°C, separation kettle II pressure is 5 MPa, 50ml of 95% ethanol is added as entrainer, and the extraction time is 2h;

[0037] After combining the extracts obtained from the separation tank I and the separation tank II, dissolve them with 10% acetic acid (v / v), filter and put them on the HP-20 resin column, wash 3 beds with water until neutral, and then use 3 beds Layer volume 15% ethanol (v / v) and 4 bed volumes 50% ethanol (v / v) were eluted, and 50% ethanol (v / v) eluate was collected and concentrated to dryness under reduced pressure;

[0038] Dissolve the solid in...

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Abstract

The invention discloses a method of utilizing supercritical CO2 extraction and macroporous resin adsorption separation to extract reserpine from rauvolfia verticillate. The technical scheme is that the method is characterized by comprising the following steps: firstly, crushing roots and barks of rauvolfia verticillate, placing the powder into a supercritical extraction kettle, carrying out supercritical extraction under a certain temperature and pressure, using ethanol as an entrainer, collecting the extract, dissolving the extract with an acidic aqueous solution, placing the solution into a nonpolar macroporous resin column, collecting the eluent containing the reserpine constituent, concentrating the eluent to form a solid, adding acetone to dissolve the solid, adding methanol to the solution to carry out crystallization, and finally recrystallizing to obtain a pure product. The method is simple in technologic process, high in operability, high in extraction efficiency, and suitable for industrialized production; the prepared reserpine is high in purity.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of medicinal active ingredients, and in particular relates to an extraction and separation method for reserpine in Rauwolfia. Background technique [0002] Rauwolfia is a plant of the genus Rauwolfia in the family Apocynaceae. It grows in tropical and subtropical regions, and it grows in Guangdong, Guangxi, and Yunnan in my country. The dried roots and stems of Rauwolfia have the effects of clearing wind and heat, reducing liver fire, reducing swelling and detoxification, and can be used to treat colds and fever, sore throat, snake bites, and bruises. Rauwolfia contains a variety of alkaloids, hundreds of which have been isolated. Among them, reserpine is an important raw material drug with clear antihypertensive effect. [0003] Currently, there are not many methods for extracting and isolating reserpine from Rauvolwolfia. In the early stage, benzene extraction was used, and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D459/00
CPCC07D459/00Y02P20/54
Inventor 杨丽李宇段迪钟鸣傅玉萍袁诚李金华
Owner GUANGZHOU HANFANG PHARMA
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