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Method for extracting tetrandrine

A technology of tetrandrine and extraction method, applied in the direction of organic chemistry, etc., can solve problems such as unenvironmental protection, and achieve the effect of saving consumption

Inactive Publication Date: 2011-01-26
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tao Shuhong et al. "Application of Macroporous Adsorbent Resin in Extracting Tetrandrine and Tetrandrine from Powdered Tetrandrine", Chinese Patent CN1850824 "Benefree Tetrandrine and Its Preparation Method", CN1903856 "A Tetrandrine The preparation methods of A and Tetrandrine have failed to avoid the use of more toxic solvents such as benzene and petroleum ether, which are still not environmentally friendly

Method used

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  • Method for extracting tetrandrine

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Effect test

Embodiment 1

[0033] Take 100g of fresh tetrandrine and crush it to 40 mesh, put it in an extraction tank, add 2g of quicklime, add 1L of 70% ethanol to soak and reflux for extraction for 2 hours, and the obtained extract is concentrated under reduced pressure to obtain an extract. Add 800ml of 1% hydrochloric acid, filter and apply to D72 macroporous cation exchange resin column for saturated adsorption, rinse out the acid solution with 0.5BV deionized water and save it for the next column, stop when it becomes neutral, and then use 0.5mol / L ammonia water The ethanol solution was used at 30 ml / min until no alkaloid reaction was detected by HPLC in the effluent eluate, and a total of 1 L of eluate was obtained. Concentrate the eluent under reduced pressure to 200ml, add 800ml of toluene for extraction, and recover the solvent from the toluene phase to obtain 1.6g of extract, which is dissolved in 16ml of acetone, heated and concentrated to 1.2ml, and the precipitated crystals are dissolved i...

Embodiment 2

[0035] Take 100g of fresh tetrandrine and crush it to 40 mesh, put it in an extraction tank, add 3g of quicklime, add 1.5L of 80% ethanol to soak and reflux for 2.5 hours, and the obtained extract is concentrated under reduced pressure to obtain an extract. Add 500ml of 2% hydrochloric acid, filter and apply to D72 macroporous cation exchange resin column for saturated adsorption, rinse out the acid solution with 0.5BV deionized water and save it for the next column, stop when it becomes neutral, and then use 0.5mol / L ammonia water The ethanol solution was used at 30ml / min until the eluate was detected by HPLC to have no alkaloid reaction, and a total of 900ml eluate was obtained. Concentrate the eluent under reduced pressure to 150ml, add 600ml of toluene for extraction, and recover the solvent from the toluene phase to obtain 1.7g of extract, which is dissolved in 30ml of acetone, heated and concentrated to 3ml, and the precipitated crystals are dissolved in 40ml of 90% ethan...

Embodiment 3

[0037] Take 100g of fresh tetrandrine and crush it to 60 mesh, put it in an extraction tank, add 5g of quicklime, add 2L of 90% ethanol to soak and reflux for extraction for 3 hours, and the obtained extract is concentrated under reduced pressure to obtain an extract. Add 600ml of 1% hydrochloric acid, filter and apply to D72 macroporous cation exchange resin column for saturated adsorption, rinse out the acid solution with 0.5BV deionized water and save it for the next column, stop when it becomes neutral, and then use 0.5mol / L ammonia water The ethanol solution was used at 30ml / min until the eluate was detected by HPLC to have no alkaloid reaction, and a total of 900ml eluate was obtained. Concentrate the eluent under reduced pressure to 120ml, add 600ml of toluene for extraction, recover the solvent from the toluene phase, and obtain 1.5g of extract, dissolve the extract in 30ml of acetone, heat and concentrate to 2ml, dissolve the precipitated crystals in 30ml of 95% ethano...

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Abstract

The invention relates to a method for extracting tetrandrine. The method comprises the following steps of: adding alkali into high-concentration ethanol for extracting, dissolving with an acid, separating with D732 macroporous cation exchange resin, extracting with toluene, and alternately crystallizing with acetone ethanol to obtain the product. The method of the invention for producing tetrandrine has the advantages of simple operation, low cost and high purity of the product.

Description

Technical field: [0001] The invention relates to a method for extracting tetrandrine, in particular to a process for preparing tetrandrine by adding alkali and alcohol, separating, extracting and crystallizing macroporous resin. Background technique: [0002] Fangji, also known as Fangji, Han Fangji, and Stone Toad, is the dry root of the perennial winding vine of Fangjiaceae Stephaniatetrandra S. Moore. The main active ingredient is alkaloid, wherein the content of tetrandrine (Tetrandrine) is 0.40-1.33%. [0003] tetrandrine [0004] Alias: tetrandrine powder, tetrandrine, tetrandrine [0005] Chemical name: (+)-Tetrandrine [0006] Molecular formula: C 38 h 42 N 2 o 6 [0007] Molecular weight: 622.76 [0008] Molecular Structure: [0009] [0010] Ingredient classification: Bisbenzylisoquinoline alkaloids [0011] Physical properties: Colorless needle crystal (ether), melting point 215-217°C, almost insoluble in water and petroleum ether, soluble in ether a...

Claims

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Application Information

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IPC IPC(8): C07D491/18
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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