Preparation and quality control method for high purity cleidion brevipetiolatum glycoside A

A quality control method, the technology of cinnamonin, which is applied in the field of preparation of high-purity cinnamonin A and its quality control, can solve the problems of low yield, high production cost, low purity of cinnamonin A, etc. Achieve the effects of fast separation speed, short production cycle and simple method

Active Publication Date: 2013-06-12
玉林市中医医院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a high-purity rod in order to overcome the existing defects of low purity, low yield or high production cost of cinnamon A, as well as the non-systematic extraction, purification and quality

Method used

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  • Preparation and quality control method for high purity cleidion brevipetiolatum glycoside A
  • Preparation and quality control method for high purity cleidion brevipetiolatum glycoside A
  • Preparation and quality control method for high purity cleidion brevipetiolatum glycoside A

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Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: Get 5 kg of leaves of Euphorbiaceae Phyllostachys chinensis, grind into below 100 orders, extract 3 times with ethanol with a volume concentration of 50%, filter, merge the filtrate, reclaim ethanol, obtain ethanol extract, obtain extractum, After silica gel column chromatography, gradient elution with chloroform-methanol volume ratio (100:0-95:5), collect the eluted part with chloroform-methanol volume ratio (95:5), detect with TCL, and collect the Fractions of A were combined and concentrated to obtain crude crystals of cinnamonin A. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: water = 22:78; detection wavelength: 255nm; flow rate: 5mL / min), and collected Glycoside A component, and each collected eluent was detected by HPLC (chromatographic column: C-18 column; mobile phase (volume ratio): acetonitrile:0.2% phosphoric acid solution=28:72; detection wavelength: 255n...

Embodiment 2

[0040] Embodiment 2: Get 5 kg of leaves of Euphorbiaceae Phytophthora barbatus, grind them into less than 100 orders, extract 4 times with 60% ethanol, filter, merge the filtrate, reclaim ethanol, obtain ethanol extract, obtain medicinal extract, pass through silica gel Column chromatography, gradient elution with chloroform-methanol (100:0~90:10), collect the eluted part with a volume ratio of chloroform-methanol (90:10), detect with TCL, collect the fraction containing cinnamonin A , combined and concentrated to obtain crude crystals of cinnamonin A. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: water = 20:80; detection wavelength: 255nm; flow rate: 5mL / min), and collected Glycoside A component, and each collected eluent was detected by HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: 0.2% phosphoric acid solution = 30:70; detection wavelength: 255nm;...

Embodiment 3

[0041] Embodiment 3: Get 5 kg of leaves of Euphorbiaceae Phyllostachys chinensis, grind them into less than 100 orders, extract 5 times with 80% ethanol, filter, merge the filtrate, reclaim ethanol, obtain ethanol extract, obtain medicinal extract, pass through silica gel Column chromatography, gradient elution with chloroform-methanol (100:0~85:15), collect the volume ratio: chloroform-methanol (85:15) eluted part, detect with TCL, collect the stream containing cinnamonin A Separated, combined, and concentrated to obtain crude crystals of cinnamonin A. The crude crystals were prepared by preparative RP-HPLC (column: C-18 column; volume ratio: mobile phase: acetonitrile: water = 25:75; detection wavelength: 255nm; flow rate: 5mL / min), and collected Glycoside A component, and each collected eluent was detected by HPLC (chromatographic column: C-18 column; mobile phase: acetonitrile: 0.2% phosphoric acid solution = 40: 60; detection wavelength: 255nm; flow rate: 1mL / min) combi...

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Abstract

Taking leaves of cleidion brevipetiolatum of Cleidion of Euphorbiaceae as raw material, the invention provides a preparation method, a detecting method and use of high purity cleidion brevipetiolatum glycoside A. The preparation method includes the steps of smashing leaves of the cleidion brevipetiolatum of the Euphorbiaceae, heating though alcohol for reflux extraction, achieving chromatography for ethanol extract through a silicagel column, eluting through chloroform-carbinol mixed solvent, detecting through thin-layer chromatography, collecting eluent containing the cleidion brevipetiolatum glycoside A, combining, reducing pressure, concentrating, obtaining cleidion brevipetiolatum glycoside A coarse crystalline particles, separating through a reverse phase silica gel C-18 column preparation efficient liquid phrase method, detecting every part of the eluent through analytical type high performance liquid chromatography, combining cleidion brevipetiolatum glycoside A compositions which are identical in reserved time and have a purity of 90-98% or more than 98% in weight , reducing pressure and concentrating to obtain the cleidion brevipetiolatum glycoside A with the purity of 90%-98% in weight and the cleidion brevipetiolatum glycoside A compositions with the purity of more than 98%, and controlling quality through the thin-layer chromatography and the liquid phrase chromatography.

Description

technical field [0001] The invention relates to the field of compound monomer preparation, in particular to a preparation and quality control method of high-purity cinnamonin A. 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. [0003] Cortiflorin A is a chemical component of phenylpropanol glycosides, one of the active components of plants, and an index component for the standard quality control of many plants and pharmaceu...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08G01N30/02G01N30/90
Inventor 刘元刘布鸣陈小刚黄艳宋志钊卢文杰文志云
Owner 玉林市中医医院
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