Novel preparation method of total flavonoids of wild euphorbia helioscopia in Greater Khingan Mountains

A technology of total flavonoids and a new method, which is applied in the field of separation and purification of total flavonoids by high-speed countercurrent chromatography, can solve the problems of low extraction purity, achieve the effects of improving extraction speed, overcoming low purity, and quick extraction

Active Publication Date: 2014-03-12
HEILONGJIANG DINGHENGSHENG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Advantages of the present invention: fast extraction, high product purity, greatly improved extraction speed, and at the same time greatly i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0019] A new method for obtaining high-purity total flavonoids by using ultra-high pressure extraction technology (ionic liquid as a solvent), polyamide coupling macroporous resin adsorption, and high-speed countercurrent chromatography separation and purification, the steps are as follows:

[0020] (1) Ultra-high pressure extraction: 1kg of lacquer whole grass is cut off, 1-octyl-3-methylimidazolium tetrafluoroborate solution with a concentration of 50% is used as a solvent, the ratio of solid to liquid is 1:8, and it is treated under 200MPA pressure for 4 minutes ;

[0021] (2) Fine filtration treatment: collect the extract, use a polytetrafluoroethylene membrane with a filtration accuracy of 0.1 μm, and perform fine filtration treatment at 60°C and a pressure of 0.2 MPa;

[0022] (3) Polyamide resin adsorption and elution:

[0023] 80-mesh polyamide powder was used, the concentration of the sample solution was controlled at 0.5mg / mL, the volume of the sample solution was 2...

Embodiment example 2

[0031] A kind of ultra-high pressure extraction technology (ionic liquid as solvent), polyamide coupling macroporous resin adsorption, then high-speed countercurrent chromatography separation and purification to obtain a new method of high-purity total flavonoids, the steps are as follows:

[0032] (1) Ultra-high pressure extraction: 2kg of the whole herb of lacquer is cut off, and 60% concentration of 1-butyl-3-methylimidazolium bromide salt solution is used as solvent, the ratio of solid to liquid is 1:10, and it is treated under 300MPA pressure for 3 minutes;

[0033] (2) Fine filtration treatment: collect the extract, use a polytetrafluoroethylene membrane with a filtration accuracy of 0.1 μm, and perform fine filtration treatment at 65°C and a pressure of 0.3 MPa;

[0034] (3) Polyamide resin adsorption and elution:

[0035] 100-mesh polyamide powder was used, the concentration of the sample solution was controlled at 1.5mg / mL, the volume of the sample solution was 3BV, a...

Embodiment example 3

[0043] A new method for obtaining high-purity total flavonoids by using ultra-high pressure extraction technology (ionic liquid as a solvent), polyamide coupling macroporous resin adsorption, and high-speed countercurrent chromatography separation and purification, the steps are as follows:

[0044] (1) Ultra-high pressure extraction: 5kg of the whole herb of lacquer was cut off, and 70% concentration of 1-hydroxyethyl-3-methylhexafluorophosphate solution was used as solvent, the ratio of solid to liquid was 1:12, and the pressure was treated at 400MPA for 2 minutes;

[0045] (2) Fine filtration treatment: collect the extract, use a polytetrafluoroethylene membrane with a filtration accuracy of 0.1 μm, and perform fine filtration treatment at 60 °C and a pressure of 0.4 MPa;

[0046] (3) Polyamide resin adsorption and elution:

[0047] 200-mesh polyamide powder was used, the concentration of the sample solution was controlled at 1.0mg / mL, the volume of the sample solution was ...

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Abstract

The invention belongs to the field of natural organic chemistry and relates to a novel method for extracting total flavonoids from wild euphorbia helioscopia in Greater Khingan Mountains and particularly relates to a novel method for extracting total flavonoids through ultrahigh pressure (ionic liquid as a solvent) extraction, polyamide coupled macroporous resin adsorption as well as separation and purification by using a high-speed counter-current chromatography. The method has the advantages that 1, ionic liquid is combined with ultrahigh pressure, so that the advantages of higher extraction speed and high efficiency are achieved; moreover, the process is simple, convenient and feasible, the effective components are sufficiently extracted, and the content of alkaloids is high; 2, a polyamide coupled macroporous resin adsorption and purification technology can be used for well enriching total alkaloids and further purifying the effective components; the resin is easy to treat, rapid in separation, low in expense and capable of realizing industrial utilization; 3, the high-speed counter-current chromatography has the advantages of flexibility in operation, high efficiency, high separation speed, large preparation amount, low expense and the like, and can be used for industrial application. By using the method, the obtained total flavonoids are high in content and high in purity up to 98.3%.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a new method for extracting total flavonoids from Daxinganling wild lacquer, in particular to a method for extracting total flavonoids using ultra-high pressure (ionic liquid as a solvent), polyamide coupling macroporous resin adsorption, high-speed A new method for separation and purification of total flavonoids by countercurrent chromatography. Background technique: [0002] Zeqi, also known as Wuduoyun and Wufengcao, is an annual or biennial herb. 10-30cm high, glabrous or only branched with slightly sparse hairs, purple-red at the base, light green at the top. Leaves alternate; obovate or spatulate, 1-3cm long, 0.7-1cm wide, slightly concave at the apex, finely serrated above the middle of the edge, sessile. Capsule spherical, about 3mm in diameter, 3-lobed, smooth. Seeds are brown, ovate, about 2mm long, with obvious raised reticulation, with white semicircular car...

Claims

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Application Information

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IPC IPC(8): A61K36/47
Inventor 张亚红曲晓颖李为海
Owner HEILONGJIANG DINGHENGSHENG PHARM CO LTD
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