Method of extracting and purifying bergenin from cissus pteroclada hayata

A technology of petracenin and Sifang rattan, which is applied in the field of natural medicine development and utilization, can solve the problems of incapable of industrial preparation, inability to recycle silica gel, and difficulty in large-scale preparation, and achieve easy recycling, easy industrial scale-up, and low cost Effect

Active Publication Date: 2015-12-23
GUANGXI NORMAL UNIV
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  • Abstract
  • Description
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Problems solved by technology

However, the current methods for purifying petracenin extracts are difficult to scale up
For example, silica gel column chromatography is a commonly used separation method in the laboratory, but silica gel cannot be recovered, and the eluent is toxic organic solvents such as petroleum ether, ethyl acetate, and chloroform, which are costly and difficult to operate, and cannot be used for industrial production; The recrystallization method must be used when the content of petracenin in the crystallization solution reaches a certain level. Ordinary petracenin extracts are difficult to crystallize before being enriched by other methods and cannot be directly purified by recrystallization.
In view of this, the current organic solvent extraction method is still at the stage of obtaining crude extracts containing petracenin, and to use this extraction method to prepare large quantities of pure petracenin, it is necessary to develop a purification method that can be industrialized and scaled up with low cost

Method used

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  • Method of extracting and purifying bergenin from cissus pteroclada hayata
  • Method of extracting and purifying bergenin from cissus pteroclada hayata
  • Method of extracting and purifying bergenin from cissus pteroclada hayata

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Experimental program
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Effect test

Embodiment 1

[0027] Add 50% ethanol solution to 500g of Si Fangteng powder, make the mass of Si Fangteng powder and the volume ratio of ethanol be 1:20, reflux extraction 1 time, each time 2h, centrifuge, filter, discard waste residue and collect to obtain filtrate, will The filtrate was concentrated while recovering the solvent. Add the concentrated solution with a concentration of 2.0 mg / mL into the AB-8 macroporous resin at a ratio of 1:1 by volume and mass of the macroporous resin for static adsorption for 8 hours, and then put it on the column. Use 2 column volumes of distilled water and 2 column volumes of 10% ethanol to remove impurities, then use 7 column volumes of 20% ethanol solution for elution, and collect the 20% ethanol eluted fraction. Concentrate the eluate to obtain 10.3 g of crude petracenin, and obtain 8.9 g of pure petracenin after recrystallization from 95% ethanol.

Embodiment 2

[0029] Add 1Kg of vine powder to 50% ethanol solution, so that the mass volume ratio of vine powder and ethanol is 1:15, reflux extraction 2 times, each 2h, centrifuge, filter, discard the waste residue to collect the filtrate, the filtrate Concentrate while recovering the organic solvent. Add the concentrated solution with a concentration of 2.0 mg / mL into the D3520 macroporous resin at a ratio of 1:1 by volume and mass of the macroporous resin for static adsorption for 8 hours, and then put it on the column. Use 2 column volumes of distilled water and 2 column volumes of 10% ethanol to remove impurities. Then use 7 times the column volume of 20% ethanol solution for elution, and collect the 20% ethanol eluted fraction. Concentrate the eluate to obtain 20.5 g of crude petracenin, and obtain 17.6 g of pure petracenin after recrystallization from 95% ethanol.

Embodiment 3

[0031] Add 10Kg of vine powder to 60% ethanol solution, make the mass volume ratio of vine powder and ethanol to be 1:10, reflux extraction 3 times, each time 2h, centrifuge, filter, discard the waste residue to collect the filtrate, the filtrate Concentrate while recovering the organic solvent. Add the concentrated solution with a concentration of 2.0 mg / mL to the D101 macroporous resin at a ratio of 1:1 by volume and mass of the macroporous resin for static adsorption for 8 hours, and then put it on the column. Use 2 column volumes of distilled water and 2 column volumes of 10% ethanol to remove impurities. Then eluted with 20% ethanol solution, and the 20% ethanol eluted part was collected. Concentrate the eluent to obtain 200.6 g of crude petracenin, and obtain 169.7 g of pure petracenin after recrystallization from 95% ethanol.

[0032] The yield of crude petracenin is about 2%, and the purity detected by HPLC is above 80%. After recrystallization with 95% ethanol, the ...

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Abstract

The invention discloses a method of extracting and purifying bergenin from cissus pteroclada hayata. The method comprises the steps that the cissus pteroclada hayata is smashed and screened, ethanol solution is added according to the mass-to-volume ratio of 1 to 8-20 for reflux extraction, solid-liquid separation is conducted to obtain filtrate, the filtrate is concentrated, macroporous resin is added into the concentrated solution for static adsorption, the macroporous resin subjected to adsorption is placed on a pillar, impurities are removed and elution is conducted with distilled water and ethanol solution in sequence, the eluant is collected and concentrated to obtain crude bergenin, and the crude bergenin is recrystallized with ethanol to obtain pure bergenin. According to the method, sources of raw materials are wide, price is low, production cost is low, production conditions are moderate, and pollution to the environment is light.

Description

technical field [0001] The invention relates to a method for extracting and purifying petracenin from Sifang vine, and belongs to the technical field of natural medicine development and utilization. Background technique [0002] Quartet vine ( Cissus Pteroclada Hayata ) belonging to the grape family ( Vitaceae ) Alpinia ( Cissus Linn. ) plant, named for its sharp square stems, branches, and petioles. Sifangteng is mainly distributed in the southern areas of my country's Guangxi, Guangdong, and Yunnan. It is rich in resources. Its nature is sour, astringent, sweet, and flat. It has a good curative effect on the treatment of rheumatic arthralgia, lumbar muscle strain, trauma, bleeding and other diseases. For example, farmers in Baise area directly mash the fresh leaves of Sifangteng for external application to stop bleeding; Baise Hospital makes Sifangteng into powder and injections to treat internal and external trauma bleeding, duodenal bleeding, gastritis and other dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
CPCC07B2200/13C07D493/04
Inventor 覃江克罗培林丹丹李怡杰杨瑞云陈家念唐煌
Owner GUANGXI NORMAL UNIV
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