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Novel method for extracting gentiopicrin from wild gentian

A technology of gentiopicroside and a new method, which is applied in the field of natural organic chemistry, can solve the problems of high operating temperature, high purity, and low yield, and achieve the effects of good selectivity, large adsorption capacity, and good thermal stability

Inactive Publication Date: 2014-04-09
DAXINGANLING GADOL SPORTS INGREDIENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In China, the solvent method is generally used to extract picrosides, which has the disadvantages of high operating temperature, low yield, and long time consumption. The difference of the present invention is that the extraction and separation method used mainly uses supercritical CO 2 Fluid extraction method, using macroporous resin to purify gentiopicroside in the later stage, the product not only has high yield, but also has high purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0018] Implementation Case 1: A method using supercritical CO 2 A new method for purifying gentiopicroside by fluid extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography, the steps are as follows:

[0019] (1) 1000g whole gentian grass is cut to 3cm and added to CO 2 In the supercritical extractor, ethanol is used as the entrainer, the volume percentage of the entrainer in the total extraction solvent is 1%, the extraction pressure is 20MPa, the temperature is 50°C, the extraction time is 100min, CO 2 The flow rate is 1mg / g crude drug min to obtain the extract;

[0020] (2) adjusting the pH value of the gentiopicroside extract treated in step (1) to 3.0 with hydrochloric acid, leaving it to stand, suction filtration, and concentrating under reduced pressure to obtain the crude gentiopicroside extract;

[0021] (3) Ultrafiltration membrane separation is adopted, the operating pressure of the membrane is 0.2MPa, the molecular weight cut...

Embodiment example 2

[0027] Implementation Case 2: A method using supercritical CO 2 A new method for purifying gentiopicroside by fluid extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography, the steps are as follows:

[0028] (1) 1000g whole gentian herb is cut to 4cm and added to CO 2 In the supercritical extractor, ethanol is used as the entrainer, the volume percentage of the entrainer in the total extraction solvent is 1%, the extraction pressure is 30MPa, the temperature is 50°C, the extraction time is 120min, CO 2 The flow rate is 1mg / g crude drug min to obtain the extract;

[0029] (2) adjusting the pH value of the gentiopicroside extract treated in step (1) to 4.0 with hydrochloric acid, leaving it to stand, suction filtration, and concentrating under reduced pressure to obtain a crude gentiopicroside extract;

[0030] (3) Ultrafiltration membrane separation is adopted, the operating pressure of the membrane is 0.2MPa, the molecular weight cut-of...

Embodiment example 3

[0036] Implementation Case 3: A method using supercritical CO 2 A new method for purifying gentiopicroside by fluid extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography, the steps are as follows:

[0037] (1) 1000g whole gentian grass is cut to 6cm and added to CO 2 In the supercritical extractor, ethanol is used as the entrainer, the volume percentage of the entrainer in the total extraction solvent is 1%, the extraction pressure is 30MPa, the temperature is 50°C, the extraction time is 120min, CO 2 The flow rate is 1mg / g crude drug min to obtain the extract;

[0038] (2) adjusting the pH value of the gentiopicroside extract treated in step (1) to 4.0 with hydrochloric acid, leaving it to stand, suction filtration, and concentrating under reduced pressure to obtain a crude gentiopicroside extract;

[0039] (3) Adopt ultrafiltration membrane to separate, membrane operating pressure is 0.2MPa, molecular weight cut off 5000, rejection ...

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Abstract

The invention belongs to the field of natural organic chemistry, relates to a method for extracting gentiopicrin from wild gentian in the Great Khingan Mountains, and in particular relates to a novel method for purifying the gentiopicrin by utilizing supercritical CO2 fluid extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography. The method has the advantages that 1, due to the application of supercritical CO2 fluid extraction, original taste and color can be prevented from being damaged by heat, heat sensitivity can be ensured, easy-to-oxidize substances can be prevented from being damaged, and extract can be separated and purified in an extraction process; 2, due to the adoption of a macroporous resin purification technology, good purification effects on active ingredients are achieved, and industrial production is facilitated; 3, ultrafiltration is finished at normal temperature, so that the structural changes, loss and biological activity of the active ingredients can be prevented from being reduced by heat effects, and the yield of the active ingredients is improved.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for extracting gentiopicroside from wild gentian in Daxing'an Mountains, in particular to a supercritical CO 2 A new method of fluid extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography purification. Background technique: [0002] Gentiana is a perennial herb, 1-2 feet tall. The leaves are opposite, the lower leaves 2-3 pairs are very small, showing scales, the middle and upper leaves are lanceolate, the surface is dark green, the back is light green, there are three obvious veins, no petiole. The flowers are born in the axils of the branches or near the tips, and have blue tube-shaped bell-shaped flowers. The fruit is oblong and slightly flattened, with two petals cracked after maturity, and the seeds are numerous and small. The rhizome is short, clustered with many slender roots, light yellowish brown or light yellow....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCY02P20/54
Inventor 万莉张亚红姚德坤
Owner DAXINGANLING GADOL SPORTS INGREDIENT
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