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Extraction method of tetrandrine and demethyltetrandrine

A technology of tetrandrine and tetrandrine, which is applied in the field of separation and extraction of effective plant components, can solve the problems that the carrier is not suitable for recycling, the process is not easy to scale up, the production environment and the hazards of operators, etc., so as to reduce the environmental and Potential harm to operators, small loss of target components, and the effect of improving raw material utilization

Inactive Publication Date: 2014-06-25
XIAN BOTANICAL GARDEN SHAANXI PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The current extraction process of tetrandrine and tetrandrine [see "Handbook of Extraction and Separation of Chemical Components of Traditional Chinese Medicine" edited by Yang Yun and Feng Weiwei, P130-133; The monomeric alkaloids in the total alkaloids] have the following problems: ①The purification process uses benzene as the purification solvent to remove tetrandrin, which not only leaves residues in the finished product, but also poses potential hazards to the production environment and operators; ②Using Silica gel or resin is the main separation carrier, the carrier is not suitable for recycling, and the operation is complicated and the production cost is high, which makes the process difficult to scale up and cannot be industrialized;

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  • Extraction method of tetrandrine and demethyltetrandrine

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Effect test

example 1

[0018] Step 1. Extract the extract: pulverize the medicinal materials of Hanfangji into 20 mesh coarse powder, take 100 kg, add 2 kg of quicklime powder and mix evenly, put it into a stainless steel multifunctional extraction tank, and add 400 kg of methanol solution with a volume concentration of 70% , heated and kept boiling for 2 hours, and filtered out the solution; then extracted twice with 300kg of 70% methanol solution according to the above method respectively, merged the obtained extracts three times, and concentrated under reduced pressure to recover methanol to obtain a total alkaloid extract with a specific gravity of 1.12;

[0019] Step 2, extraction for the first time: the obtained extract is dissolved at 35° C. with a 5% concentration of hydrochloric acid aqueous solution to make it an acidic aqueous solution with pH 2, and a mixture of ethyl acetate and chloroform (volume ratio 1:5) is used to dissolve the extract. The mixed solvent is used as the extraction so...

example 2

[0023] Step 1. Extract the extract: crush 200kg of Hanfangji medicinal materials into 40 mesh coarse powder, add 5kg of quicklime powder and mix evenly, put it into a stainless steel multifunctional extraction tank, add 800kg of ethanol solution with a volume concentration of 80%, and heat Keep boiling for 2 hours, filter out the solution; then extract twice by the above-mentioned method with 600kg 80% ethanol solution respectively, combine the obtained extracts three times, concentrate under reduced pressure to recover ethanol, and obtain a total alkaloid extract with a specific gravity of 1.15;

[0024] Step 2, the first extraction: dissolve the extract obtained in step 1 with a 2% concentration of sulfuric acid aqueous solution at 35 ° C to make it into an acidic aqueous solution with a pH of 2.5, and use chloroform as an extraction solvent to extract the acidic aqueous solution. The tetracycline was detected by TLC at the same time, until there was no obvious reaction spot ...

example 3

[0028] Step 1. Extract the extract: add 500kg of 50-mesh Hanfangji medicinal material coarse powder, add 15kg of quicklime powder and mix evenly, put it into a stainless steel multifunctional extraction tank, add 2000kg of ethanol solution with a volume concentration of 85%, and keep it boiling by heating 2 hours, filter out the solution; then extract twice by the above-mentioned method with the 85% ethanol solution of 1500kg respectively, merge the obtained extracts three times, and concentrate under reduced pressure to reclaim ethanol to obtain a total alkaloid extract with a specific gravity of 1.15;

[0029]Step 2, the first extraction: the extract obtained in step 1 is dissolved in a phosphoric acid aqueous solution with a concentration of 2% at 60 ° C to make it into an acidic aqueous solution with a pH of 2.5, and chloroform is used as an extraction solvent to extract the Han in the acidic aqueous solution. At the same time, TLC was used to detect the tetragonine until t...

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Abstract

The invention relates to an extraction method of tetrandrine and demethyltetrandrine. The extraction method comprises the steps of: uniformly mixing Stephania tetrandra powder and quick lime powder, carrying out alcohol extraction to obtain total alkaloid extract, adjusting the pH value to 2-4, extracting, and standing for layering; carrying out alkalization and reduction on the extract liquid to obtain extract, dissolving the extract in acetone, filtering, concentrating and crystallizing to obtain tetrandrine crude product, and recrystallizing the tetrandrine crude product to obtain a tetrandrine product; and adjusting pH value of the acidic aqueous solution obtained after standing to 9-11, extracting to obtain extract, dissolving the extract in acetone, filtering, concentrating and crystallizing to obtain demethyltetrandrine crude product, and recrystallizing the demethyltetrandrine crude product to obtain a demethyltetrandrine product. Compared with the prior art, the extraction method has the advantages that: the characteristics of the solubility difference between free tetrandrine and free demethyltetrandrine and demethyltetrandrine salts generated by reaction between acid and each of tetrandrine and demethyltetrandrine is utilized, tetrandrine and demethyltetrandrine can be separately obtained by adjusting the pH value; the operation controllability is good, the component loss is low, the extractant can be reused, benzene is not used in extraction process, and the production cost is low; the extraction method is suitable for industrial production; tetrandrine and demethyltetrandrine products can be simultaneously obtained; and the raw material utilization rate is effectively improved and the production cost is lowered.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction of plant effective components, and in particular relates to a method for extracting sulfamethoxine A and sulfamethoxine B from fenugreek. Background technique [0002] Tetrandrine (Tetrandrine, also known as tetrandrine, powder tetrandrine) and Demethyl-tetrandrine (Demethyl-tetrandrine, also known as demethyl-tetrandrine, tetrandrine) are derived from tetrandrine. Bisbenzylisoquinoline alkaloids isolated from the roots of the plant Hanfangji (also known as Fenfangji, Shibufo, Baimuxiang, Stephania tetrandra S.Moore), the structural formula is as follows. [0003] [0004] Tetrandrine Demethyl-tetrandrine [0005] At present, there are many pharmacological studies on proteoglycan, and tablets and injections have been used in clinical practice as anti-rheumatic drugs and anti-cancer synergistic drugs for rheumatism, arthralgia, neuralgia and other diseases. Combined with low-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/18
Inventor 周军辉王答祺李思锋李静
Owner XIAN BOTANICAL GARDEN SHAANXI PROV