Preparation method and quality detecting method of high-purity phlorizin

A high-purity technology for phlorizin, which is applied in the field of preparation of high-purity phlorizin and its quality inspection, and can solve the problems of unreached purity and inability to meet high-purity phlorizin chemical reference substances

Active Publication Date: 2019-12-06
GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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Problems solved by technology

Some separation methods have high separation purity, but most of the purity does not meet the requirements of traditional Chinese medicine chemical reference substances, that is, the purity is greater than 98%, which cannot meet the needs of high-purity phlorizin chemical reference substances; Composition determination is the main focus, but there are no related reports on the quality control and evaluation of phloridizin chemical reference substances

Method used

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  • Preparation method and quality detecting method of high-purity phlorizin
  • Preparation method and quality detecting method of high-purity phlorizin
  • Preparation method and quality detecting method of high-purity phlorizin

Examples

Experimental program
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Effect test

Embodiment 1

[0116] A preparation method for high-purity phlorizin, specifically comprising the steps of:

[0117] 1) 1 kg of dry leaf powder of Acaeaceae, reflux extraction with 10 times the weight of ethanol with a volume concentration of 70% for 3 times, filter the extract, combine the filtrates, recover the ethanol, and obtain the extract;

[0118] 2) Extract the extract with petroleum ether, let it stand, discard the petroleum ether layer, extract the water part with ethyl acetate, let it stand, combine the ethyl acetate layer, and concentrate to obtain the ethyl acetate extract;

[0119] 3) The ethyl acetate extract was chromatographed on a silica gel column and eluted with a methanol-dichloromethane system gradient to collect fractions containing phlorizin. The gradient elution conditions of the methanol-dichloromethane system were: 0- 5min, the elution system is dichloromethane; 5-15min, the elution system is methanol-dichloromethane, the volume ratio of methanol:dichloromethane is...

Embodiment 2

[0128] A preparation method for high-purity phlorizin, specifically comprising the steps of:

[0129] 1) 1 kg of dried leaf powder of Fructus Polycarpa, reflux extraction with 5 times the weight of ethanol with a volume concentration of 70% for 4 times, filter the extract, combine the filtrates, reclaim the ethanol, and obtain an extract;

[0130] 2) Extract the extract with petroleum ether, let it stand, discard the petroleum ether layer, extract the water part with ethyl acetate, let it stand, combine the ethyl acetate layer, and concentrate to obtain the ethyl acetate extract;

[0131] 3) The ethyl acetate extract was chromatographed on a silica gel column and eluted with a methanol-dichloromethane system gradient to collect fractions containing phlorizin. The gradient elution conditions of the methanol-dichloromethane system were: 0~ 8 minutes, the elution system is dichloromethane; 8-20min, the elution system is methanol-dichloromethane, the ratio of methanol:dichloromethan...

Embodiment 3

[0140] A preparation method for high-purity phlorizin, specifically comprising the steps of:

[0141] 1) 1 kg of dry leaf powder of Fructus Polycarpus is extracted 5 times with 50% ethanol at a volume concentration of 8 times the weight, the extract is filtered, the filtrate is combined, and the ethanol is reclaimed to obtain an extract;

[0142] 2) Extract the extract with petroleum ether, let it stand, discard the petroleum ether layer, extract the water part with ethyl acetate, let it stand, combine the ethyl acetate layer, and concentrate to obtain the ethyl acetate extract;

[0143] 3) The ethyl acetate extract was chromatographed on a silica gel column and eluted with a methanol-dichloromethane system gradient to collect fractions containing phlorizin. The gradient elution conditions of the methanol-dichloromethane system were: 0~ 5 minutes, the elution system is dichloromethane; 5-15min, the elution system is methanol-dichloromethane, the ratio is 1:100; 15-40min, the e...

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Abstract

The invention relates to a preparation method and quality detecting method of high-purity phlorizin. The preparation method comprises the steps that dried leaf powder of lithocarpus polysachyus (DC.)rehd. is subjected to reflux extraction through ethyl alcohol, extracting solutions are combined and concentrated, suspension is extracted through petroleum ether, then the water liquid part is takenand extracted through ethyl acetate, an ethyl acetate layer is taken and concentrated, and thus an extract is obtained; the ethyl acetate extract is subjected to silica-gel column chromatography, subjected to gradient elution through a methanol-dichloromethane system and detected through thin-layer chromatography, eluent containing the phlorizin is collected and combined, vacuum concentration is conducted, then gel column chromatography is conducted, elution is conducted through a methanol-trichloromethane system, eluent containing the phlorizin is collected, vacuum concentration is conducted,and recrystallization is conducted to obtain phlorizin coarse crystallization; and then separation and purification are conducted through preparation-high performance liquid chromatography (HPLC), the collected eluent is detected through HPLC, and thus the phlorizin with the purity being within 90-98% and a phlorizin composition with the purity being greater than 98% are obtained. According to the preparation method, a technology is simple, the separation speed is high, the production period is short, the obtained product is high in purity, the quality is controllable, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of extracting phlorizin from traditional Chinese medicine plants, in particular to a method for preparing high-purity phlorizin and its quality detection method. Background technique [0002] Chemical reference substances, also known as standard substances, are physical controls for research on quality standards of traditional Chinese medicine, quality testing and quality control. Research on chemical reference substances of traditional Chinese medicine is a very important part of standardization research of traditional Chinese medicine. In the quality control of pharmaceutical production, chemical reference substances of traditional Chinese medicine play an extremely important role, and are the basis and core of quality control of traditional Chinese medicine. Phlorizin is a flavonoid chemical component, the chemical name is 1-(2-(β-D-glucopyranoseoxy)-4,6-dihydroxyphenyl)-3-(4-hydroxyphenyl) - Acetone, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H15/203G01N30/06G01N30/86G01N30/90
CPCC07H1/08C07H15/203G01N30/06G01N30/8631G01N30/90
Inventor 袁健童刘布鸣柴玲黄艳冯军陈明生
Owner GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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