Method for extracting high-purity esculine and fraxin from Cortex Fraxini

A kind of technology of aricin and aricin, which is applied in the fields of aricin and aricin, can solve the problems of difficult crystallization and high viscosity, and achieve the effects of low production cost, high product yield and easy control of production scale

Inactive Publication Date: 2015-01-28
XIAN BOTANICAL GARDEN SHAANXI PROV
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AI-Extracted Technical Summary

Problems solved by technology

The main problem of this method is that the solution to be crystallized contains a large amount of plant...
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Abstract

The invention provides a method for extracting high-purity esculine and fraxin from Cortex Fraxini, which comprises the following steps: pulverizing a Cortex Fraxini raw material and extracting under hot reflux by a conventional process, preparing a dual-water phase, dissolving, extracting, concentrating, desalinizing and crystallizing. The method mainly comprises the following steps: 1) preparing a dual-water phase system, and separating to obtain an upper phase and a lower phase for later use, and dissolving a Cortex Fraxini extract in the upper phase solvent; 2) centrifugating or filtering the solution containing the Cortex Fraxini extract, adding a right amount of lower phase solvent, sufficiently stirring and mixing, standing, separating the upper phase solution, and concentrating, thereby effectively removing inorganic substances, monosaccharides, polysaccharides. vegetable proteins, chlorophyl and other solid impurities in the Cortex Fraxini extract and enhancing the contents of esculine and fraxin; and removing salts and other impurities from the solution by conventional processes, and concentrating to a proper concentration, thereby sequentially obtaining the esculine and fraxin crystals. The method solves the problems of low crystallizing tendency, high production cost, complex operation and the like in the existing process of preparing esculine and fraxin from Cortex Fraxini, and has the characteristics of simple production equipment, environment friendliness and the like.

Application Domain

Sugar derivativesSugar derivatives preparation

Technology Topic

SolventCortex Fraxini +9

Image

  • Method for extracting high-purity esculine and fraxin from Cortex Fraxini
  • Method for extracting high-purity esculine and fraxin from Cortex Fraxini
  • Method for extracting high-purity esculine and fraxin from Cortex Fraxini

Examples

  • Experimental program(1)

Example Embodiment

[0028] Below in conjunction with example the present invention is described in further detail. For the TLC and HPLC detection methods in the examples, refer to "Workbook of Chemical Reference Substances of Traditional Chinese Medicine" edited by Chen Dechang (China Medical Science and Technology Press, 2000, P129‐130).
[0029] Take 1 kg of Qinpi medicinal material (origin: Shaanxi), crush it into coarse powder, add 6 kg of ethanol, heat to reflux for 1 hour, and filter out the solution; then add 4 kg of ethanol and heat to reflux for 1 hour, filter out the solution, and combine the two extracts , concentrating under reduced pressure and recovering ethanol to obtain an extract with a specific gravity of 1.15 for subsequent use.
[0030] Keep the ambient temperature at 20°C, prepare a two-phase aqueous system with ammonium sulfate, ethanol, and water (the mass concentrations of ammonium sulfate and ethanol in the system are 14% and 30%, respectively), and after fully mixing, let it stand until the volume of the upper and lower phases is no obvious. Change, separate the upper and lower phase solutions, set aside.
[0031] Adopt a small amount of multiple times, fully dissolve the extract with the above-mentioned upper phase solution, detect with TLC or HPLC, until there is no obvious auretin in the extract, the test results are as follows: figure 1 , figure 2 and image 3 shown. Combine the above solutions to a total of 4.2 liters, add 0.5 liters of the lower phase solution to extract the solution twice, until the proportion of solid impurities in the upper phase solution is no longer significantly reduced. Separate the upper phase containing the solution of auretin and arugeretin, concentrate under reduced pressure to 0.2 liters, add ethanol until the alcohol content is above 90%, remove inorganic salts, then concentrate under reduced pressure to remove ethanol, add appropriate amount of water to the obtained solution and heat to dissolve , stand still, crystallize, and filter to obtain 16.8 g of the crude product of fencoletin, which is recrystallized with ethanol to obtain 8.6 g of white fencoletin with a purity of 98.6%; Glycoside crystals and a small amount of ethanol were placed again, crystallized, and filtered to obtain 6.8 g of light yellow auvetin needle crystals with a purity of 98.2%.

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