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Traditional Chinese medicine venenum bufonis extract and preparation method thereof

A technology of extract and toad venom, applied in the field of traditional Chinese medicine toad venom extract and its preparation, can solve the problems of low extraction efficiency, increased toxicity, and low content, and achieve the effects of reducing dust pollution, increasing purification purity, and simplifying purification methods

Active Publication Date: 2012-06-27
北京协和制药二厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent application "a kind of toad venom extract and preparation method thereof" (application number is 200710041880.7, publication number is CN101322723A, announcement date is December 17, 2008) uses dehydrated alcohol to extract, and extract is separated through silica gel column, with certain The method of isocratic elution with the ratio of petroleum ether and acetone obtains a mixture of three fat-soluble components of esterbufagenin, cinobufagin and bufafolin, the total amount of which is higher than 90%, but the method adopts an extraction solvent of Dehydrated alcohol, its extraction efficiency is lower, and the consumption of sherwood oil used for separation, acetone is bigger, and the degree of environmental pollution and destruction is also bigger; investigation, and the transfer rate has not been disclosed; more importantly, this method does not specify the drying temperature and time of the traditional Chinese medicine Bufoni extract, because organic solvents are used in the separation and purification process, which may lead to A large amount of toxic organic solvents such as petroleum ether and acetone remain, resulting in low content and greatly increased toxicity
Therefore, from the perspective of safety and effectiveness, the total content of the three bufagenins needs to be further increased, and the residual amount of organic solvents such as acetone and petroleum ether has not been checked and measured.

Method used

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  • Traditional Chinese medicine venenum bufonis extract and preparation method thereof
  • Traditional Chinese medicine venenum bufonis extract and preparation method thereof
  • Traditional Chinese medicine venenum bufonis extract and preparation method thereof

Examples

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Effect test

Embodiment 1

[0034]Take 1 gram of toad venom medicinal material, grind it finely through a 30-mesh sieve, add 15 mL of ethanol aqueous solution with a volume percentage of 75%, reflux extraction at 80°C for 60 minutes, extract twice under the above conditions, combine the filtrate, and filter the extract while it is hot , After concentration by rotary evaporation, add 1.2 grams of silica gel for mixing samples to obtain silica gel for mixing samples. Adopt separation column 1, take 12 grams of separation silica gel, take sherwood oil and acetone (volume ratio is 3: 1) as eluent, first soak this separation silica gel with 40mL of eluent for 1 hour, then wet-pack the column, add the The obtained mixed sample silica gel was then eluted isocratically with eluent for 60 minutes. Monitor by thin layer chromatography, collect the eluate containing the three bufoginins, evaporate to dryness, and dry under reduced pressure at 35° C. for 12 hours to obtain the extract of the traditional Chinese medi...

Embodiment 2

[0036] Take 10g of toad venom herb, grind it finely through a 60-mesh sieve, add 100mL of 85% ethanol aqueous solution by volume, reflux extraction at 80°C for 45 minutes, extract 3 times under the above conditions, combine the filtrates, and filter the extracts while they are hot. After rotary evaporation and concentration, 13.0 g of silica gel for mixing samples was added to obtain the mixing sample silica gel. Adopt separation column 1, get 150 grams of separation silica gel, take sherwood oil and acetone (volume ratio is 4: 1) as eluent, first soak this separation silica gel with 300mL of eluent and then wet pack the column after 1 hour, add the The mixed sample silica gel obtained was then eluted isocratically with the eluent. Monitored by HPLC, collect the eluate containing the three bufoginins, evaporate to dryness, and dry under reduced pressure at 45° C. for 60 hours to obtain the extract of the traditional Chinese medicine Bufondin of the present invention. Wherein,...

Embodiment 3

[0038] Take 5g of toad venom herb, grind it finely through a 20 mesh sieve, add 60mL of 90% ethanol aqueous solution by volume, reflux and extract at 90°C for 30 minutes, extract 3 times, combine the filtrate, filter the extract while it is hot, concentrate it by rotary evaporation, and then add 5.0 grams of mixed samples are mixed with silica gel to obtain mixed samples of silica gel. Adopt separation column 1, get 50 grams of separation silica gel, take sherwood oil and acetone (volume ratio is 3: 1) as eluent, first soak this separation silica gel with 130mL of eluent and then wet pack the column after 1 hour, add the The mixed sample silica gel obtained was then eluted isocratically with the eluent. Monitored by HPLC, collect the eluate containing the three bufoginins, evaporate to dryness, and dry under reduced pressure at 40° C. for 60 hours to obtain the extract of the traditional Chinese medicine toad venom of the present invention. Wherein, the weight percentage of t...

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Abstract

The invention relates to a traditional Chinese medicine venenum bufonis extract. A method for extracting the extract includes steps of extracting traditional Chinese venenum bufonis medical materials at the temperature ranging from 60 DEG C to 90 DEG C by ethanol water with volume percent of 60-95% in a backflow manner, separating extract liquid via silicagel columns after the extract liquid is concentrated, adopting petroleum ether and acetone with volume ratio of 1-8:1 as eluant to realize gradient elution, collecting parts of eluent, and filtering, concentrating and drying the eluent in a pressure reduction manner to obtain the traditional Chinese medicine vanenum bufonis extract containing mixture of three types of bufotalin including resibufogenin, cinobufagin and bufalin, wherein the sum of the weight percentages (calculated when three types of the bufotalin are dried) of the three types of the bufotalin is higher than or equal to 95%. The invention further provides the preparation method for the traditional Chinese medicine venenum bufonis extract. The sum of the weight percentages of the three types of the bufotalin in the traditional Chinese medicine venenum bufonis extract is higher than 95%, extraction transfer rate is high, the quantity of used solvent is lower, residual solvent is little, pollution degree is lower, operation is simple and convenient, and industrial production is realized easily.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine extraction, and in particular relates to a traditional Chinese medicine toad venom extract and a preparation method thereof. Background technique [0002] The medicinal toad is Bufo bufogaraarizans Cantor or Bufo meLanostictus Schneider, which is an animal of the amphibian bufo family. Toad venom is the white slurry secreted by the auricular glands and skin glands of the giant bufo or black-framed toad, which is processed and dried. The application of traditional Chinese medicine toad venom has a history of thousands of years. The description of toad venom in "Compendium of Materia Medica" is as follows: toad venom travels through twelve meridians, Tibet, membranes, valleys, and joints. Toad venom is also a medicine for treating malnutrition accumulation, dispelling swelling and detoxifying furunculosis. It can dissolve all stagnant and stagnant diseases, such as accumulatio...

Claims

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Application Information

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IPC IPC(8): A61K35/56A61P35/00A61K35/65
Inventor 何秀峰刘冬赵立敏
Owner 北京协和制药二厂有限公司
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