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Extraction method of tetrandrine and demethyltetrandrine

A technology of fenacetin A and fenacetin B, applied in the field of separation and extraction of plant active components, can solve the problems that carriers are not suitable for recycling, the process is not easy to enlarge, and the production cost is high, so as to reduce the potential of the environment and operators. Harm, improve the utilization rate of raw materials, the effect of small loss of target components

Inactive Publication Date: 2012-03-21
XIAN BOTANICAL GARDEN SHAANXI PROV
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  • Claims
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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;

Method used

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  • Extraction method of tetrandrine and demethyltetrandrine

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example 1

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

[0019] Step 2, extraction for the first time: the hydrochloric acid aqueous solution of gained extract is dissolved at 35 ℃ with the hydrochloric acid aqueous solution of 5% concentration, makes it become the acidic aqueous solution that pH is 2, with ethyl acetate and chloroform (volume ratio 1: 5) The mixed solvent is used as the extraction solvent to extract the tetrand...

example 2

[0023] Step 1. Extraction extract: crush 200kg of Hanfangji medicinal material 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 use 600kg of 80% ethanol solution to extract twice according to the above method, combine the extracted solution obtained three times, concentrate under reduced pressure and 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 2% sulfuric acid aqueous solution at 35°C to make it an acidic aqueous solution with a pH of 2.5, and use chloroform as the extraction solvent to extract the acidic aqueous solution Tetrandrine, at the same time detected by TLC, until there is no obvious tetrandrine reaction spots in the acidic aqueous...

example 3

[0028] Step 1. Extract the extract: add 500 kg of 50-mesh Chinese Fangji medicinal material coarse powder, add 15 kg of quicklime powder and mix evenly, put it into a stainless steel multifunctional extraction tank, add 2000 kg of ethanol solution with a volume concentration of 85%, and heat to keep boiling 2 hours, filter out solution; Then extract twice with the 85% ethanol solution of 1500kg respectively according to the above-mentioned method, merge three times gained extracts, concentrating under reduced pressure reclaims ethanol, obtains the total alkaloid extract that specific gravity is 1.15;

[0029]Step 2, the first extraction: dissolve the extract obtained in step 1 with a 2% phosphoric acid aqueous solution at 60°C to make it an acidic aqueous solution with a pH of 2.5, and use chloroform as the extraction solvent to extract Han in the acidic aqueous solution. Tetrandrine is detected by TLC method at the same time until there is no obvious tetrandrine reaction spot ...

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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 tetrandrine and tetrandrine from Fang. Background technique [0002] Tetrandrine (Tetrandrine, also known as Tetrandrine, Tetrandrine) and Demethyl-tetrandrine (also known as Tetrandrine, Tetrandrine, Tetrandrine) are from the The bisbenzylisoquinoline alkaloid isolated from the root of the family plant Hanfangji (also known as Fenfangji, Shibufa, Baimuxiang, Stephania tetrandra S. Moore) has the following structural formula. [0003] [0004] Tetrandrine Demethyl-tetrandrine [0005] At present, there are many pharmacological studies on tetrandrine. Tablets and injections have been used clinically as antirheumatic drugs and anticancer synergistic drugs for rheumatism, arthralgia, neuralgia and other diseases. Combined application of low-dose radiation in the treatment of lung cancer is also ...

Claims

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Application Information

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