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A kind of preparation method of gentiopicroside in Gentiana flavus

A technology of chopicroside and Gentipicroside coarse powder, which is applied in the field of preparation of gentiopicroside in Gentiana chrysanthemum, can solve the problems of limited raw material range of gentiopicroside, difficult process control, complicated process technology, etc., and achieve the protection of endangered plants Resources, low production costs, and the effect of expanding the range of raw materials

Active Publication Date: 2018-12-18
GANSU UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a preparation method of gentiopicroside in Gentiana flavinaceae, to solve the problems of limited range of gentiopicroside raw materials, complicated process technology, difficult process control and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 200g of Gentiana japonica coarse powder, add 2000ml of 95% ethanol, extract at 60°C for 3 hours, filter to remove insoluble impurities, distill the filtrate to recover ethanol to obtain the extract, dry the extract at 80°C, and obtain 42g of dry extract with a moisture content of no more than 20% Then the gentiopicroside crude extract is dissolved in 95% ethanol with 400ml volume percentage concentration, and activated carbon is added according to 35% (14.7g) of the gentiopicroside crude product weight, after reflux decolorization, filter, and reclaim ethanol under reduced pressure, The crystals just precipitated, kept in refrigerator at 4°C for 3 days, filtered to obtain 7.2 g of gentiopicroside, with a purity of 90.3% (HPLC external standard method), added 95% ethanol to the crude crystals to make a hot saturated solution, and suction filtered while it was hot. Store in refrigerator at 4°C for 1 day, filter, and recrystallize 3 times with 95% ethanol in the same w...

Embodiment 2

[0032] Take 200g of Gentiana japonica coarse powder, add 3000ml of acetone, reflux and extract at 57°C for 3 hours, filter to remove insoluble impurities, distill the filtrate to recover acetone to obtain the extract, dry the extract at 90°C, and obtain 39g of dry extract with a moisture content of not more than 20% ; Dissolve the crude extract of gentiopicroside with 1000ml propanol, add activated carbon according to 25% (9.75g) of the crude product weight of gentiopicroside, after reflux decolorization, filter, recover acetone under reduced pressure, just precipitate crystals, and store in the refrigerator Refrigerated at 4°C for 4 days, filtered to obtain 8.2g of gentiopicroside, with a purity of 91.1%, adding acetone to the crude crystals to make a hot saturated solution, suctioning and filtering while hot, refrigerated at 4°C for 2 days, filtered, The above method was used to recrystallize 4 times with acetone to obtain a gentiopicroside product with a purity of more than ...

Embodiment 3

[0034] Take 200g of Gentiana japonica coarse powder, add 2500ml of propanol, extract at 50°C for 4 hours, filter to remove insoluble impurities, distill the filtrate to recover propanol to obtain the extract, dry the extract at 80°C, and obtain 45g of dry extract with a moisture content of not more than 20% matter; then dissolve the crude gentiopicroside extract with 900ml propanol, add activated carbon according to 30% (13.5g) of the crude product weight of gentiopicroside, after reflux decolorization, filter, recover propanol under reduced pressure, and just precipitate crystals , kept in refrigerator at 4°C for 5 days, and filtered to obtain 7.5 g of gentiopicroside with a purity of 90.9%. Add propanol to the crude crystals to make a hot saturated solution, suction filter while it is hot, store in refrigerator at 4°C for 1 day, filter, and recrystallize 5 times with propanol in the same way as above to obtain a purity of more than 99% (HPLC external standard method) of gent...

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Abstract

The purpose of the invention is to provide a preparation method of gentiopicroside in Gentiana officinalis in order to solve the problems of limited gentiopicroside raw material range, complicated technology, difficulty process control and high cost. The preparation method comprises the steps of extraction, drying, decolorizing and re-crystallization. The preparation method of gentiopicroside, adopting the Gentiana officinalis as a raw material, has the advantages of enlargement of the raw material range, low device requirements, easiness in process control, technology simplification and low production cost, the purity of the obtained gentiopicroside reaches 90% or above, gentiopicroside with the purity of 98% or above is obtained after re-crystallizing the gentiopicroside with an organic solvent 3-5 times, and the high performance liquid chromatography (HPLC external standard method) detected purity is 99% or above.

Description

technical field [0001] The invention belongs to the technical field of natural medicines, and in particular relates to a preparation method of gentiopicroside from Gentiana flavette. Background technique [0002] At present, the preparation of gentiopicroside mostly adopts the method of combining solvent extraction and chromatographic separation. The crude extract of gentiopicroside is extracted from the original plant, and the crude extract is separated by silica gel column chromatography, and mixed solvents such as chloroform and methanol with a certain volume ratio Elution, repeated separation and collection of gentiopicroside. [0003] Another method is to crush the original plant, add a certain amount of aqueous solution to heat and extract 2-3 times, the extract is absorbed by the macroporous resin, the eluate is concentrated by nanofiltration membrane, and the concentrated solution is purified by polyamide column, ethyl acetate Extraction, concentration and crystalli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 赵磊李冲彭雪晶夏鹏飞
Owner GANSU UNIV OF CHINESE MEDICINE
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