Method for separating and refining arteannuin, dihydro-artemisinic acid and artemisinic acid by reversed-phase high performance liquid chromatography

A reversed-phase high-efficiency liquid phase, dihydroartemisinic acid technology, applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., can solve the problems of discarding and resource waste, achieve large sample loading, increase production, and reduce The effect of production costs

Inactive Publication Date: 2011-08-17
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the current artemisinin extraction method only obtains a small amount of artemisinin, and most of the compounds that can be converted into artemisinin or have high value themselves are discarded, resulting in a great waste of resources

Method used

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  • Method for separating and refining arteannuin, dihydro-artemisinic acid and artemisinic acid by reversed-phase high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 100g dry sample of Artemisia annua, add 800mL of petroleum ether, reflux and extract at 60°C for 3 times, each time for 1h, combine the extracts, filter, and recover petroleum ether in vacuo to obtain 4.6g of crude extract, add 1.15mL of acetonitrile to resuspend, vacuum Suction filtration, the filtrate is passed through a 0.45 μm microporous filter membrane, and the preparative high-performance liquid chromatography adopts the following preparative chromatographic conditions: with Shimadzu PRC-ODS, reversed-phase column, internal diameter 20mm, length 250mm; Mobile phase is acetonitrile / water ( The volume ratio is 60:40); the flow rate is 15 mL / min; the detection wavelength is 192 nm; the column temperature is 40° C.; the injection volume is 400 μL. At the same time, artemisinin, artemisinic acid and dihydroartemisinic acid standards were prepared into solutions, and the artemisinin, artemisinic acid and dihydroartemisinic acid determined under the same chromatogr...

Embodiment 2

[0023] Weigh 200g of dried Artemisia annua, add 1.6L of petroleum ether, reflux and extract at 60°C for 3 times, each time for 1h, combine the extracts, filter, and recover petroleum ether in a vacuum to obtain 9.4g of crude extract, add 2.35mL of acetonitrile to resuspend, Vacuum suction filtration, pass the filtrate through a 0.45 μm microporous membrane, and apply the preparative high-performance liquid chromatography, using the following preparative chromatographic conditions: use Shimadzu PRC-ODS, reversed-phase column, inner diameter 30mm, length 250mm; mobile phase is acetonitrile / water (The volume ratio is 60:40), the flow rate is 40 mL / min; the detection wavelength is 192 nm; the column temperature is 40° C.; the injection volume is 800 μL. At the same time, artemisinin, artemisinic acid and dihydroartemisinic acid standards were prepared into solutions, and the artemisinin, artemisinic acid and dihydroartemisinic acid determined under the same chromatographic conditio...

Embodiment 3

[0025] Weigh 500g dry sample of Artemisia annua, add 4L petroleum ether, reflux and extract at 60°C for 3 times, each time for 1h, combine the extracts, filter, and recover petroleum ether in vacuo to obtain 24.6g crude extract, add 6.15ml acetonitrile to resuspend, vacuum Suction filtration, pass the filtrate through a 0.45 μm microporous filter membrane, and put it on a preparative high-performance liquid chromatography column, adopt the following preparation chromatographic conditions: use Shimadzu PRC-ODS, reversed-phase column, internal diameter 50mm, length 250mm; mobile phase is acetonitrile / water (The volume ratio is 60:40), the flow rate is 100 mL / min; the detection wavelength is 192 nm; the column temperature is 40° C.; the injection volume is 2 mL. At the same time, artemisinin, artemisinic acid and dihydroartemisinic acid standards were prepared into solutions, and the artemisinin, artemisinic acid and dihydroartemisinic acid determined under the same chromatographi...

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Abstract

The invention relates to a method for separating and refining arteannuin, dihydro-artemisinic acid and artemisinic acid by reversed-phase high performance liquid chromatography. The method mainly comprises the following steps of: separating and purifying an artemisia apiacea crude extract extracted by organic solvent by reversed-phase high performance liquid chromatography, and concentrating and crystallizing to obtain pure products of the arteannuin, the dihydro-artemisinic acid and the artemisinic acid. The method is high in yield, separation efficiency and a separation speed, the pure products of the arteannuin, the dihydro-artemisinic acid and the artemisinic acid can be obtained simultaneously, and the purity can reach over 96 percent, so the method can be used for large-scale industrial production.

Description

Technical field: [0001] The present invention relates to a method for separating and refining artemisinin, artemisinic acid and dihydroartemisinic acid from Artemisia annua extract, in particular to a method for separating and refining artemisinin, artemisinin and dihydroartemisinin by reverse-phase high-performance liquid chromatography Methods of Artemisinic Acid and Artemisinic Acid. Background technique: [0002] According to the latest report of the World Health Organization, malaria has become the most widespread, longest history, and most harmful human parasitic infectious disease. It has long been one of the diseases with the highest morbidity and mortality in third world countries. At present, there are 300-500 million clinical cases in the world every year, of which more than 1 million deaths. With global warming and environmental damage, the incidence of malaria has been on the rise in recent years. The traditional antimalarial drugs quinine and sulfonamide have...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20C07C33/14C07C29/76
Inventor 刘硕谦刘仲华田娜黄建安
Owner HUNAN AGRICULTURAL UNIV
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