Preparation and quality control method of high-purity cinnamon a

A technology of clavenosides and clavenosides is applied in the field of preparation and quality control of high-purity clavenosides A, and can solve the problems of low yield, high production cost, low purity of clavenosides A, and the like, Achieve the effect of fast separation speed, short production cycle and simple and easy method.

Active Publication Date: 2015-09-23
玉林市中医医院
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  • Summary
  • 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 control method Preparation of pachinoside A and its quality control method, the method prepared by the method is high in purity and good in quality, and can be used as a chemical reference substance or standard substance to ensure quality control

Method used

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  • Preparation and quality control method of high-purity cinnamon a
  • Preparation and quality control method of high-purity cinnamon a
  • Preparation and quality control method of high-purity cinnamon a

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Example 1: Take 5 kg of the leaves of Euphorbiaceae plant stalk flower, crush it into 100 meshes or less, extract 3 times with ethanol with a volume concentration of 50%, filter, combine the filtrate, and recover the ethanol to obtain an ethanol extract to obtain an extract. After silica gel column chromatography, eluted with a chloroform-methanol volume ratio (100:0~95:5) gradient, collect the chloroform-methanol volume ratio (95:5) elution fraction, detect with TCL, and collect the clavicle The fractions of A were combined and concentrated to obtain crude crystals of stalk anthocyanin 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 collect the flowers Glycoside A component, and use HPLC to detect each collected eluate (chromatographic column: C-18 column; mobile phase (volume ratio): acetonitrile: 0.2% phosphoric ...

Embodiment 2

[0039] Example 2: Take 5 kg of the leaves of Euphorbiaceae stalk flower, crush it to below 100 mesh, extract 4 times with 60% ethanol, filter, combine the filtrate, recover the ethanol to obtain the ethanol extract, obtain the extract, and pass it through silica gel Column chromatography, eluted with a gradient of chloroform-methanol (100:0~90:10), collected the elution fraction with a volume ratio of chloroform-methanol (90:10), detected by TCL, collected the fractions containing clavin A , Combined and concentrated to obtain crude crystals of C. 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 collect the flowers Glycoside A component, and use HPLC to detect each collected eluate (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: 0.2% phosphoric acid solution = 30:70; detection wavelength: 255nm;...

Embodiment 3

[0040] Example 3: Take 5 kg of the leaves of Euphorbia spp. stalk flower, crush it to below 100 mesh, extract 5 times with 80% ethanol, filter, combine the filtrate, recover the ethanol to obtain the ethanol extract, obtain the extract, and pass it through silica gel Column chromatography, eluted with a gradient of chloroform-methanol (100:0~85:15), collected the volume ratio: chloroform-methanol (85:15) elution fraction, detected with TCL, collected the flow containing clavicularin A Separate, combine, and concentrate to obtain crude crystals of C. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: water=25:75; detection wavelength: 255nm; flow rate: 5mL / min), and collect the flowers Glycoside A component, and use HPLC to detect each collected eluate (chromatographic column: C-18 column; mobile phase: acetonitrile: 0.2% phosphoric acid solution = 40: 60; detection wavelength: 255 nm; flow rate...

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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 method for the preparation of high-purity clerotin A and its quality control. Background technique [0002] Chemical reference substance, also known as standard substance, is the physical control of the quality standard research, quality inspection and quality control of Chinese medicine. The research of Chinese medicine chemical reference substance is a very important part of the standardization research of Chinese medicine. In the quality control of pharmaceutical production, the chemical reference substance of traditional Chinese medicine plays an extremely important role and is the basis and core of the quality control of traditional Chinese medicine. [0003] Clavinoside A is a chemical component of phenylpropanol glycoside compounds, one of the active components of plants, and an indicator component for standard quality control of many plants and medicines. At presen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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