Method for extracting esculetin from herba violae

A technology of escin and viola, which is applied in the direction of organic chemistry, etc., can solve the problems that are not suitable for industrial production, and achieve good results

Inactive Publication Date: 2011-05-18
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such methods are not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Crush the raw material of Viola dichotoma, take 1kg, add 10kg of 60% ethanol to reflux and extract twice, extract for 2 hours each time, filter to obtain the extract, recover the ethanol under reduced pressure, add HZ806 (resin 500ml) to the large pores after diluting the concentrated solution with water The resin column is adsorbed. After the adsorption is completed, the resin column is washed with water until it is sugar-free, and then 3L of 50% ethanol is taken to elute the active ingredient. The eluent is recovered from the ethanol, and the pH is adjusted to 1 with 10% hydrochloric acid solution while it is still hot. The precipitate is filtered out. Ethyl acetate was refluxed to dissolve, peracid alumina short column (alumina 120-300 mesh, dosage 80g), the column liquid was recovered to 1 / 5 volume and placed to crystallize, the crystal was filtered out, 60% ethanol was refluxed and dissolved, and then concentrated to 1 / 3 volume crystallized twice, the crystals were...

Embodiment 2

[0023] Crush the raw material of Viola dichotoma, take 1 kg, add 7 kg of 90% ethanol to reflux extraction for 3 times, extract for 1 hour each time, filter, extract the ethanol under reduced pressure, dilute the concentrated solution with water, add LSA-7 (resin 600ml) Porous resin column adsorption, after the adsorption is completed, first wash the resin column with water until it is sugar-free, then take 2.4L of 80% ethanol to elute the active ingredient, recover the ethanol from the eluent, adjust the pH to 3 with 10% hydrochloric acid solution while it is hot, and place the precipitate, filter the precipitate out, ethyl acetate reflux to dissolve, peracid aluminum oxide conventional column (alumina 120-300 mesh, dosage 100g), the column liquid is recovered to 1 / 6 volume and placed to crystallize, and the crystal is filtered out, and after 90% ethanol reflux dissolves Concentrate to 1 / 5 volume of crystals, filter out the crystals, and dry to obtain 1.8 g of pale yellow cryst...

Embodiment 3

[0025] Take Viola dichotoma raw material, take 10kg, put it into a 500L stainless steel extraction tank, add 100kg of 80% ethanol to reflux extraction twice, extract for 2 hours each time, filter, extract the extract under reduced pressure to recover ethanol, add ADS- 17 (resin 5L) macroporous resin column adsorption, after the adsorption is completed, first wash the resin column with water until it is sugar-free, then take 25L of 65% ethanol to elute the active ingredients, recover the ethanol from the eluent, and adjust the pH1 with 10% hydrochloric acid solution while it is hot Precipitate, precipitate is filtered out, ethyl acetate is refluxed to dissolve, peracid alumina conventional column (alumina 120-300 mesh, dosage 1kg), the column liquid is recovered to 1 / 4 volume and placed for crystallization, and the crystallization is filtered out, 80 % ethanol was refluxed to dissolve, concentrated to 1 / 3 volume and crystallized twice, the crystals were filtered off, and dried t...

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Abstract

The invention relates to a method for extracting esculetin from herba violae. The method comprises the following steps: using herba violae as a raw material to grind, adding 7-15 times of 60-90% ethanol to perform backflow extraction for 2-3 times; filtering, recycling ethanol under reduced pressure, diluting the concentrated solution with hot water; adding macroporous resin for adsorption; washing resin column with water to ensure that the solution has no caramel colour; using 4-6 BV of 50-80% ethanol to elute the active ingredient, recycling ethanol from eluent; adjusting the acidity of the hot solution for precipitation, filtering out the precipitate, dissolving the precipitate with ethyl acetate through refluxing; adding the solution in an aluminum peroxide column, recycling the obtained solution in a small-column container, and standing for crystallization; dissolving the obtained crystals with ethanol to perform refluxing and recrystallization; and drying the obtained crystals to obtain the esculetin product. By adopting the method to produce esculetin, the technology is simple, is easy to operate, has low production cost and high product purity.

Description

Technical field: [0001] The invention relates to a method for extracting aescin, in particular to a method for extracting aescin from Viola chinensis. Background technique: [0002] Escinolide is a coumarin compound, also known as aricetin, the chemical name is 6,7-dihydroxycoumarin, yellow needle crystal (alcohol), mp.268-270°C. Soluble in methanol, ethanol and sodium hydroxide solution, soluble in ethyl acetate and acetone solution, slightly soluble in boiling water, almost insoluble in ether, chloroform and water. [0003] Escinolide has antibacterial, anti-inflammatory and antitussive and expectorant effects, and has a good therapeutic effect on bacillary dysentery and acute enteritis. [0004] Existing extracts of escin are mostly extracted and prepared from Aesculetin. Since Aescin also contains similar substances such as aescin, aescin and aescin, the purification is relatively difficult and the production cost is relatively high. The process route is to extract the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/16
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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