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Incarvillateine preparation method

A technology of artemisinin and artemisia, applied in the field of natural medicinal chemistry, can solve the problems of serious production pollution, complicated operation and high production cost

Inactive Publication Date: 2013-12-11
NANJING TONGZE AGRI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing method for preparing carartemisinic acid has technical defects such as serious production pollution, high production cost, and complicated operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take the raw material of Artemisia annua and crush it, weigh 5kg, add 8 volumes of 70% ethanol solution to reflux and extract 3 times, combine the extracts and concentrate to a density of 1.2 and release, add 500ml of 5% hydrochloric acid aqueous solution to the extract and stir thoroughly, filter out insolubles, and use ammonia water as the filtrate Adjust the pH to 12, add 500ml chloroform solution to extract 3 times, recover chloroform from the extract, add 300g neutral alumina reagent to dry and pulverize, place in a supercritical CO2 extraction tank for extraction, the CO2 flow rate is 3ml / min / g raw material, and the extraction temperature is 40°C , pressure 18Mpa, extraction time 3h, analysis extract 80% methanol solution was refluxed, dissolved and recrystallized 3 times, and the crystal was dried to obtain 18g of carotene base, which was detected by HPLC with a content of 98.1%.

Embodiment 2

[0014] Take Artemisia annua raw material and crush it, weigh 5kg, add 7 volumes of 80% ethanol solution to reflux and extract 3 times, combine the extracts and concentrate to a density of 1.15 and release, add 800ml of 5% hydrochloric acid aqueous solution to the extract and stir well, filter out insoluble matter, and use ammonia water as the filtrate Adjust pH11, add 700ml chloroform solution to extract twice, recover chloroform from the extract, add 400g neutral alumina reagent to dry and pulverize, place in supercritical CO2 extraction tank for extraction, CO2 flow rate is 2ml / min / g raw material, extraction temperature is 50°C , pressure 22Mpa, extraction time 3h, analysis of the extract 75% methanol solution was refluxed, dissolved and recrystallized 3 times, and the crystal was dried to obtain 19g of carotene base, which was detected by HPLC with a content of 96.3%.

Embodiment 3

[0016] Take Artemisia annua raw material, weigh 5kg, add 10 volumes of 90% ethanol solution to reflux and extract twice, combine the extracts and concentrate to a density of 1.2 and release, add 500ml of 5% hydrochloric acid aqueous solution to the extract and stir thoroughly, filter out insoluble matter, and use ammonia water as the filtrate Adjust the pH to 12, add 500ml chloroform solution to extract 3 times, recover chloroform from the extract, add 300g neutral alumina reagent to dry and pulverize, place in a supercritical CO2 extraction tank for extraction, the CO2 flow rate is 4ml / min / g raw material, and the extraction temperature is 45°C , pressure 20Mpa, extraction time 3h, analysis extract 80% methanol solution was refluxed, dissolved and recrystallized 3 times, and the crystal was dried to obtain 16g of carotene base, which was detected by HPLC with a content of 97.7%.

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PUM

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Abstract

The invention discloses an incarvillateine preparation method which is simple and convenient to operate and low in pollution. The incarvillateine preparation method comprises the following steps of: crushing an incarvillea raw material, adding 5-10 times amount of 50-80% ethanol solution for reflux extraction two to three times, recovering a reagent from an extracting solution, adding a right amount of 5% hydrochloric acid aqueous solution to extract, filtering, carrying out ammoniation on filtrate, extracting by using a chloroform solution, recovering the reagent from extract liquor, adding a right amount of aluminium oxide reagent for drying and crushing, and placing in a supercritical CO2 extraction tank for extraction, wherein the CO2 flow rate is 1-4ml / min / g raw material, the extraction temperature is 30-60 DEG C, the pressure is 15-30Mpa, and the extraction time is 1-4h; refluxing, dissolving and recrystallizing a resolved extract by using a methanol solution two to three times, and drying crystals, thus obtaining the incarvillateine. The incarvillateine preparation method is simple in process, low in production cost and easy for realizing industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a preparation method of carrageenate base. Background technique [0002] Artemisinin is a monoterpene alkaloid, molecular formula C11H21NO, insoluble in petroleum ether and water, soluble in chloroform, benzene, ether, and acidic water, soluble in methanol, ethanol and acetone. Carrageenate base has strong analgesic activity, and its mechanism of action is different from that of morphine. Artemisinin has become a new drug for the development of new non-narcotic analgesics. [0003] Artemisia annua is a plant of Bignoniaceae, which is commonly used for expelling wind and dampness, promoting blood circulation and relieving pain, and detoxifying. The main chemical components are alkaloids, cyclohexyl alcohols, coumarins, iridoids, flavonoids and so on. [0004] Through literature search: the existing methods for extracting artemisinin from Artemisia annua ge...

Claims

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Application Information

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IPC IPC(8): C07D221/04
CPCY02P20/54
Inventor 杨存
Owner NANJING TONGZE AGRI SCI & TECH