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Method for preparing 3, 3', 4', 5, 7-pentumethoxyflavone in melicope triphylla

A technology of pentamethoxyflavone and trefoil honey, which is applied in the field of natural medicinal chemistry, can solve the problems of cumbersome operation and unsuitability for industrial preparation, and achieve the effects of reducing pollution, low cost and high product quality

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cornus officinalis, also known as soft-shelled turtle, is a shrub, produced in Taiwan (Hengchun Peninsula, Lanyu), and also in the Philippines. It has been reported that a variety of highly oxidized flavonoids were isolated from Cornus three-leaf, but The operation is cumbersome and not suitable for industrial preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take the leaves of Cornus officinalis Trifoliata and dry them at low temperature, weigh 5kg and degrease them twice with 5 times the amount of petroleum ether, 1 hour each time, evaporate the degreased medicinal materials to dry the residual reagents, add 75% ethanol and soak at 50°C for 24 hour, extract 2 times, filter, combine the filtrates, concentrate to obtain the extract, then add acetone and ammonium sulfate and mix evenly, so that the volume of acetone in the formed two-phase system is 18% of the amount of extract, and the quality of ammonium sulfate accounts for 18% of the total liquid 15% of the volume, shaking in a water bath at 55°C for 1 hour, standing for 3 hours to separate the phases, taking out the upper phase of acetone rich in flavonoids from Trifoliate Fructus Corni, adding ethyl acetate, dipotassium hydrogen phosphate, water, fully Mix well, let stand at 25°C for 5 hours, take out the ethyl acetate phase, concentrate under reduced pressure to recover...

Embodiment 2

[0014] Take the leaves of Cornus officinalis Trifoliata and dry them at low temperature, weigh 5kg and degrease them twice with 5 times the amount of petroleum ether, 1 hour each time, evaporate the degreased medicinal materials to dry the residual reagents, add 60% ethanol and soak at 50°C for 36 hour, extract 2 times, filter, combine the filtrates, concentrate to obtain the extract, then add acetone and ammonium sulfate and mix evenly, so that the volume of acetone in the formed two-phase system is 21% of the amount of extract, and the quality of ammonium sulfate accounts for the total liquid 18% of the volume, shake in a water bath at 55°C for 1 hour, let stand for 3 hours to separate phases, take out the upper phase of acetone rich in flavonoids of Mitsuba officinalis, add ethyl acetate, ammonium sulfate, water, and mix well , let stand at 30°C for 6 hours, take out the ethyl acetate phase, concentrate under reduced pressure to recover the reagent, add silica gel short and ...

Embodiment 3

[0016] Take the leaves of Cornus officinalis and dry them at low temperature, weigh 10kg and degrease them twice with 5 times the amount of petroleum ether, 1 hour each time, evaporate the degreased medicinal materials to dry the residual reagents, add 80% ethanol and soak at 50°C for 12 hour, extracted 3 times, filtered, combined filtrates, concentrated to obtain extract, then added acetone and ammonium sulfate and mixed evenly, so that the volume of acetone in the formed two-phase system was 12% of the amount of extract, and the quality of ammonium sulfate accounted for the total liquid 20% of the volume, shake in a water bath at 50°C for 1 hour, let stand for 3 hours to separate the phases, take out the upper phase of acetone rich in flavonoids of Mitsuba Flavone, add ethyl acetate, dipotassium hydrogen phosphate, water, fully Mix well, let stand at 20°C for 3 hours, take out the ethyl acetate phase, concentrate under reduced pressure to recover the reagent, add silica gel s...

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PUM

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Abstract

The invention discloses a method for preparing 3, 3', 4', 5, 7-pentumethoxyflavone in melicope triphylla and belongs to the field of natural medicine chemistry. The method comprises the steps: taking, drying and crushing melicope triphylla leaves, degreasing with petroleum ether, carrying out warm immersion on a degreased medical material with 60-80 percent of ethanol, concentrating a filtrate to obtain an extract, adding into an acetone and ammonium sulfate double-water phase system in proportion to uniformly mix, dividing into an upper phase and a lower phase, taking an acetone phase rich in melicope triphylla flavone, adding water, ethyl acetate and inorganic salt for back extraction, concentrating an ethyl acetate phase under reduced pressure, carrying out silica-gel column chromatography, and recrystallizing methylene dichloride-acetone to obtain the 3, 3', 4', 5, 7-pentamethoxyl flavone. The method has the advantages of economy and high extraction rate and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and relates to a method for preparing 3,3',4',5,7-pentamethoxyflavone from cornus officinalis. Background technique [0002] 3,3’,4’,5,7-Pentamethoxyflavone (3,3’,4’,5,7-Pentumethoxyflavone) is pale yellow plate-like crystal with molecular formula C 20 h 20 o 7 , molecular weight 372.37, mp.150-151°C. Exist in a variety of plants, such as Rutaceae honey dogwood Melicope triphylla Merr.'s leaf, Verbenaceae plant Duhonghua Callicarpa formosana Rolfe's Leaf and Zingiber officinale Boesenbergia pandurata (Roxb.) Schltr. in the rhizome, etc. Cornus officinalis, also known as soft-shelled turtle, is a shrub, produced in Taiwan (Hengchun Peninsula, Lanyu), and also in the Philippines. It has been reported that a variety of highly oxidized flavonoids were isolated from Cornus three-leaf, but The operation is cumbersome and not suitable for industrial preparation. 3,3',4',5,7-pentame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH