Method for preparing tetrandrine alkaloids by coupling in-situ conversion-adsorptive separation technology

A technology of adsorption separation and total alkaloids, which is applied in the direction of medical preparations containing active ingredients, digestive system, drug combination, etc., and can solve problems such as complex methods, loss of resin advantages, and complex process operations

Inactive Publication Date: 2009-12-23
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following main problems: 1) most processes in the extraction need to use a large amount of highly toxic solvents such as benzene and chloroform in an open environment, which is very harmful to operators and the environment; 2) the sample loss is more during activated carbon decolorization; 3 ) method is complicated, operability is poor, and production cost is higher
Wang Mingkui etc. disclose a kind of method (Wang Mingkui, Cui Wenfeng, Bao L

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 25g of the commercially available tetrandrine was crushed, and it was incubated with 75mL of 80% (v%) ethanol solution at 45°C and stirred for 2.5h, and extracted 4 times under the same conditions. Combine the four filtrates, distill under reduced pressure to recover ethanol, add 5% (v%) acetic acid aqueous solution to a solution volume of 75 mL, filter, and adjust the pH of the filtrate to 10 with ammonia water. The precipitate is dissolved in a 5% (v%) acetic acid aqueous solution, centrifuged, and the supernatant is collected, which is the adsorption solution (wherein, the total alkali content of tetrandrine is 31.6%, w%).

[0018] Pack the column with X-5 resin (column diameter is 17mm, column length is 190mm, resin volume is 25mL), and 75mL of the above adsorption solution is passed through the resin column at a speed of 1BV / h. After the adsorption is completed, the resin bed is washed with a large amount of deionized water , Then use 2BV of 5% (w%) ammonia water, 3BV ...

Embodiment 2

[0020] 133g of the commercially available tetrandrine was crushed, and was incubated with 400mL of 85% (v%) ethanol solution at 50°C and stirred for 2h, and extracted 3 times under the same conditions. Combine the three filtrates, distill under reduced pressure to recover ethanol, add an aqueous solution containing 4% (v%) of acetic acid to a solution volume of 400 mL, filter, and adjust the pH of the filtrate to 12 with ammonia water. The precipitate is dissolved in 6% (v%) acetic acid aqueous solution, centrifuged, and the supernatant is collected, which is the adsorption solution (wherein, the total alkali content of tetrandrine is 33.2%, w%).

[0021]Pack the column with X-5 resin (column diameter is 20mm, column length is 350cm, resin volume is 100mL), 400mL of the above adsorption solution is passed through the resin column at a speed of 2BV / h, after the adsorption is completed, a large amount of deionized water is used for the resin bed Wash, and then wash the resin column ...

Embodiment 3

[0023] 500g of commercially available tetrandrine was pulverized, and heated and stirred at 60°C for 3h with 2000mL of 90% (v%) ethanol water, and extracted 5 times under the same conditions. Combine the 5 filtrates, distill under reduced pressure to recover ethanol, add 6% (v%) acetic acid aqueous solution to a solution volume of 1500 mL, filter, and adjust the pH of the filtrate to 10 with ammonia water. The precipitate is dissolved in 8% (v%) acetic acid aqueous solution, centrifuged, and the supernatant is collected, which is the adsorption solution (wherein, the total alkali content of tetrandrine is 30.4%, w%).

[0024] Pack the column with X-5 resin (column diameter is 55mm, column length is 60cm, resin volume is 500mL), and 1500mL of the above adsorption solution is passed through the resin column at a speed of 3BV / h. After the adsorption is completed, a large amount of deionized water is used for the resin bed Cleaning, followed by rinsing the resin column with 4BV 6% (w%...

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Abstract

The invention relates to a method for preparing tetrandrine alkaloids by coupling in-situ conversion-adsorptive separation technology, and the preparation process comprises: 1) tetrandrine raw drug is ground and soaked into ethanol water solution for heat preservation and agitation. After the mixed solution is filtered, filtrate is processed by reduced pressure distillation, and ethanol is recovered; acetic acid water solution is added into the processed filtrate which is then filtered, ammonia water is used for adjusting the pH value of the filtrate to be within the range of 10-12, and precipitate is separated out; the obtained precipitate is dissolved into the acetic acid water solution and centrifugated, and supernate is collected and called as adsorption solution for short; 2) after the adsorption solution with the quantity being 3-5 times of bed volume is absorbed by resin column, a resin bed layer is washed by a great quantity of deionized water, and then the tetrandrine alkaloids extract is obtained by the steps such as using the ammonia water to pass through the resin column, etc. In the preparation process, noxious solvent is not used, and other solvents are consumed in a small quantity; meanwhile, resin is not needed to be processed by acid-alkali regeneration after the extraction period of every time, so that the operation technique is greatly simplified, the resin can be reused, a great deal of resources can be saved, the extraction efficiency is improved, and the method is suitable for industrialized large-scale production. The prepared tetrandrine alkaloids have the purity being higher than 70% and the yield being higher than 95%.

Description

【Technical Field】: [0001] The invention relates to the technical field of extraction and separation of effective components of traditional Chinese medicine, in particular to a method for preparing total alkaloids of tetrandrine by in situ conversion-adsorption separation technology combined. 【Background technique】: [0002] Tetrandrine is the root of Stephania tetrandra S.Moore, a plant of the genus Stephania tetrandra S. Moore in the tetrandrine family. It has a long history of clinical use in my country. The main active ingredient is alkaloids, such as tetrandrine (also known as tetrandrine). ), fangchinoline (also known as tetrandrine, demethyltetrandrine), methyl tetrandrine, diberberamine, ring cylinol and so on. Among them, tetrandrine A and tetrandrine B have the highest content, and they are also the main medicinal ingredients in tetrandrine. [0003] The plant of the genus Stephania has long been anti-cancer in our country. Among them, tetrandrine has a preventive effect...

Claims

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Application Information

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IPC IPC(8): A61K36/59A61P35/00A61P11/00A61P9/12A61P1/16A61P9/10A61P27/02A61P29/00A61K125/00
Inventor 王春红施荣富麻宁夏建军
Owner NANKAI UNIV
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