Production process for extracting, separating and purifying potentilla flavone

A technology of separation and purification and Potentilla, which is applied in the fields of sugar derivatives, sugar derivatives, organic chemistry, etc., and can solve problems such as difficulty in ensuring effective ingredients

Inactive Publication Date: 2010-06-16
TIANJIN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Through extraction and separation, it is still difficult to ensure that active ingredients with high purity can be obtained, and it is necessary to select an appropriate purification method to purify the separated substances

Method used

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  • Production process for extracting, separating and purifying potentilla flavone
  • Production process for extracting, separating and purifying potentilla flavone
  • Production process for extracting, separating and purifying potentilla flavone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 25kg of naturally dried and crushed Chinese herbal Potentilla Potentilla produced in Ji County, Tianjin, add 200kg of 60% ethanol to soak overnight, heat and reflux for extraction for 1.5 hours, filter, then reflux extract with 150kg of 60% ethanol for 1.5 hours, filter; then add 150kg of 60% ethanol to extract Reflux extraction for 1.5 hours, combine the three extracts, and concentrate to obtain 4.6 kg of extract, the content of flavonoids in Potentilla spinach was determined to be 4.050‰ by HPLC.

[0023] The above extract was dissolved in 46kg 30% ethanol, fully stirred, centrifuged at 3000r / min for 10min, the supernatant was taken, separated with 20-60 mesh AB-8 macroporous adsorption resin column, 10BV was loaded, and the adsorption flow rate was 2BV / h. Then eluted with 30% ethanol at a mass concentration of 3BV, 60% ethanol at a mass concentration of 5BV, and 95% ethanol at a mass concentration of 4BV, and the elution flow rate was 2BV / h, and the 60% ethanol e...

Embodiment 2

[0026] Take 30kg of naturally dried and pulverized traditional Chinese medicine Potentilla from Jixian County, Tianjin, add 240kg of 60% ethanol to soak overnight, heat and reflux for extraction for 1.5 hours, filter, then reflux with 180kg of 60% ethanol for 1.5 hours, filter; then reflux with 180kg of 60% ethanol After extracting for 1.5 hours, the three extracts were combined and concentrated to obtain 5.4 kg of extract, in which the flavonoid content of Potentilla flavonoids was 4.022‰. Dissolve in 54kg30% ethanol, stir well, centrifuge at 3000r / min for 10min, take the supernatant, separate it with 20-60 mesh AB-8 macroporous adsorption resin column, load 10BV, the adsorption flow rate is 2BV / h, and then sequentially with 3BV Elute with 30% ethanol at a mass concentration, 60% ethanol at a mass concentration of 5BV, and 95% ethanol at a mass concentration of 4BV. Liquid A (the content of flavonoids in the extract is 3.4%). Dissolve the resulting suspension in an equal vol...

Embodiment 3

[0029] Take 35kg of naturally dried and pulverized traditional Chinese medicine Potentilla from Jixian County, Tianjin, add 280kg of 60% ethanol to soak overnight, heat and reflux for extraction for 1.5 hours, filter, then reflux with 210kg of 60% ethanol for 1.5 hours, filter; then reflux with 210kg of 60% ethanol After extracting for 1.5 hours, the three extracts were combined and concentrated to obtain 6.1 kg of liquid extract, of which the flavonoid content of Potentilla chinensis was 4.502‰. Dissolve in 61kg of 30% ethanol, stir well, centrifuge at 3000r / min for 10min, take the supernatant, separate it with AB-8 macroporous adsorption resin column, load 10BV, the adsorption flow rate is 2BV / h, and then sequentially use 3BV mass concentration 30% Ethanol, 5BV mass concentration 60% ethanol, 4BV mass concentration 95% ethanol elution, elution flow rate 2BV / h, collect 60% ethanol eluent, concentrate under reduced pressure to no alcohol smell, the suspension A obtained (the ex...

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Abstract

The invention discloses a process for extracting, separating and purifying potentilla flavones, namely a chemical composition with antidiabetic effect in Chinese medicament potentilla, and belongs to the technology of extracting and separating active ingredients of Chinese medicaments. The compound has the following structure; and the process for extracting, separating and purifying the compound comprises the following steps: grinding the potentilla, adding 60 percent ethanol, heating, refluxing and extracting for three times in a solid-liquid ratio of 8:6:6, filtering, combining filter liquor, and evaporating and concentrating under reduced pressure to obtain an extract substance; dissolving the extract substance with 30 mass percent ethanol of which the weight is 10 times that of the extract substance, centrifuging at a rate of 3,000r / min, separating supernate with a 20- to 60-mesh AB-8 macroporous resin absorption column, making a sample volume 10BV (10 times of the column volume) and adsorption flow rate and elusion flow rate 2BV / h, eluting with 3BV of 30 percent ethanol and 5BV of 60 percent ethanol in turn, collecting eluent of the 60 percent ethanol, concentrating under reduced pressure until no alcohol smell exists, and obtaining a mixed suspension A; dissolving the mixed suspension with equal volume of 30 percent ethanol, centrifuging, separating supernate with 80- to 100-mesh polyamide chromatographic column, making a sample volume 10BV and adsorption and elusion flow rate 2BV / h, eluting with 3BV of 30 percent ethanol and 5BV of 60 percent ethanol in turn, collecting eluent of the 60 percent ethanol, concentrating under reduced pressure until no alcohol smell exists, and obtaining a mixed suspension B; centrifuging the mixed suspension B, purifying centrifuged precipitate with a high speed countercurrent chromatography, wherein in a solvent system, a ratio (volume ratio) of methylene dichloride to methanol to water is 5 to 4 to 2.

Description

technical field [0001] The invention relates to a production process for extracting, separating and purifying the flavonoids of Potentilla vulgaris Potentilla, an anti-diabetic active ingredient of Potentilla vulgaris, belonging to the field of extraction and separation of effective components of traditional Chinese medicines. Background technique [0002] Potentilla chinesis Ser., also known as Chinese cabbage, pulsatilla, toad grass, and azure, is the whole herb of Potentilla chinesis Ser., a plant in the family Rosaceae. Based on the clinical application of the traditional Chinese medicine Potentilla chinensis, this laboratory isolated and identified a compound with anti-diabetic effect from the traditional Chinese medicine Potentilla chinensis (the following formula) by means of traditional Chinese medicine chemistry and pharmacology. Metformin is equivalent and has high clinical application value. The invention relates to a production process for extracting, separating...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08A61K31/7048A61P3/10
Inventor 段宏泉赵川
Owner TIANJIN MEDICAL UNIV
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