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Preparation method of arcapillin

A technique for arginine and ethanol, applied in directions such as organic chemistry, can solve the problems such as no report on the preparation process of high-purity arginine, and achieve the effects of being beneficial to large-scale production operations, low in energy consumption, and low in pollution

Inactive Publication Date: 2012-12-05
YANGZHOU YIYANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process suitable for the industrialized large-scale production of high-purity artemisinin

Method used

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  • Preparation method of arcapillin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 10Kg of the dry aboveground part of Artemisia caprifolia, add 65% ethanol to percolate, the percolation speed is 1ml / g crude drug min, collect 30L percolation liquid, filter, recover ethanol under reduced pressure and concentrate, add to D101 macroporous adsorption Adsorbed on the resin column, eluted with 35% ethanol, collected 3 times of column volume eluate, reclaimed ethanol under reduced pressure and concentrated, added to nylon 66 (polyhexamethylene adipamide) polyamide chromatography column, calculated by ratio 4:1 ethyl acetate-methanol mixed solvent is used as eluent for elution, and the same type of polyamide film is used as a supporting test to develop with the above eluent, and the corresponding Rf=4-4.5 on the polyamide film is collected. Fractions, recovery of solvent, addition of methanol to crystallize, separation of crystals, washing and drying to obtain 12.3 g of yellow needle crystals - capcarinin, detected by HPLC, the purity is 93.3%, UV, IR, MS...

Embodiment 2

[0027] Take 10Kg of the dry aboveground part of Artemisia chinensis, add 80% ethanol for percolation, the percolation rate is 3ml / g crude drug min, collect 80L percolation liquid, filter, recover ethanol under reduced pressure and concentrate, add to D102 macroporous adsorption Adsorbed on the resin column, eluted with 65% ethanol, collected 8 times of column volume eluate, recovered ethanol under reduced pressure and concentrated, added to nylon 66 (polyhexamethylene adipamide) polyamide chromatographic column, and calculated according to the ratio 4:1 ethyl acetate-methanol mixed solvent is used as eluent for elution, and the same type of polyamide film is used as a supporting test to develop with the above eluent, and the corresponding Rf=4-4.5 on the polyamide film is collected. Fractions, recovered solvent, added methanol to crystallize, separated the crystals, washed and dried to obtain 14.2 g of yellow needle crystals - capcarinin, detected by HPLC, the purity was 92.0%,...

Embodiment 3

[0029] Take 10Kg of the dry aerial part of Artemisia capriculum, add 75% ethanol for percolation, the percolation speed is 2ml / g crude drug·min, collect 60L percolation liquid, filter, recover ethanol under reduced pressure and concentrate, add to AB-8 large Adsorb on the porous adsorption resin column, elute with 50% ethanol, collect 5 times of column volume eluate, reclaim ethanol under reduced pressure and concentrate, add on nylon 6 (polycaprolactam) polyamide chromatography column, with the ratio of 4: The ethyl acetate-methanol mixed solvent of 1 is eluted as eluent, develops with above-mentioned eluent with polyamide film of the same kind as supporting detection, collects the fraction corresponding to Rf=4-4.5 on the polyamide film, The solvent was recovered, methanol was added to crystallize, the crystals were separated, washed, and dried to obtain 13.6 g of yellow needle crystals-capillary artemisinin, which was detected by HPLC with a purity of 95.5%, UV, IR, MS, 2 H...

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Abstract

The invention relates to a preparation method of arcapillin, which has the advantages of simple operation, small pollution and low energy consumption. The method comprises the following process steps of: taking dried overground part of artemisia capillaris, adding ethanol percolation, collecting a percolation liquid, filtering, recycling ethanol by reducing pressure and concentrating, adding the ethanol on a macropore absorption resin column for absorption, eluting with the ethanol, collecting an eluent, recycling the ethanol by reducing pressure and concentrating, adding the ethanol on a polymide chromatographic column, eluting by taking a mixed solvent consisting of ethyl acetate and methanol in terms of the ratio of the ethyl acetate to the methanol being 4:1 as an eluant, collecting the eluent, recycling the solvent, adding the methanol to crystallize, separating and crystallizing, washing and drying to obtain the arcapillin. The arcapillin prepared with the method has high product purity and is easy to realize industrialized enlargement.

Description

technical field [0001] The invention relates to a preparation method of capillary wormwood, in particular to a preparation method of extracting capillary wormwood from plants. Background technique [0002] Arcapillin, molecular formula: C 18 h 16 o 8 , molecular weight: 360.32, CAS accession number: 83162-82-7. It is mainly found in Artemisia capillaris Thunb., a plant of Compositae, and the source of raw materials is abundant. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that artemisinin has a strong hepatoprotective effect, and it is also used as a raw material for the synthesis of other active derivatives. [0005] The dry aerial part of Artemisia capillaris Thunb., a plant of Compositae, is used as a traditional Chinese medicine Artemisia capillaris Thunb. It has the effects of clearing dampness and heat and reducing jaundice. [0006] In the prior art, there is no report on the preparation process suitable for the large-scale...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 王峰王琳张发成
Owner YANGZHOU YIYANG PHARMA