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Preparation method of trifolirhizin

A technology of trilobite pteroside and acid water, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of low product purity, small preparation amount, long cycle, etc., and achieve solvent system Simple, short separation time, high resolution effect

Inactive Publication Date: 2012-08-29
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the document "Research on Chemical Components of Nitraria japonica" published by Wen Min et al., the method disclosed in this document is 75% ethanol reflux extraction, extraction with ethyl acetate after concentration, silica gel column chromatography on the extract, and petroleum ether -Acetone mixed solvent system for elution, the eluent is then subjected to silica gel column chromatography, and eluted with a chloroform-methanol mixed solvent system, and the eluent is finally subjected to gel column chromatography to obtain trilobin with higher purity. There are many steps in the method, the amount of eluent is large, the amount of preparation is small, and the cycle is long; another example is Zhu Lijun's master's thesis "Chemical Research on the Effective Parts of Sophora Sophorae". The method used in this paper is ethanol reflux extraction. The supernatant was removed by centrifugation, the residue was separated by a silica gel column, chloroform-methanol gradient elution, the target eluent was collected, the solvent was recovered, and finally recrystallized with chloroform to obtain trilobalin. The steps of this method are relatively simple but the product purity is not tall
The existing methods for extracting pterostaloside generally have problems such as large amount of toxic organic solvents, many process steps, less preparation amount, and low product purity. Therefore, it is very important to provide a method for preparing pteroside with high purity. necessary

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 1Kg of Sophora flavescens, crush it, add 10L of 40% methanol to heat and reflux for extraction twice, combine the extracts, concentrate to obtain 62g of extract, add 310ml of pH 1 hydrochloric acid aqueous solution to the extract for ultrasonic dispersion, remove the acid water layer by centrifugation, and repeat the acid extraction of solids. Wash twice with water, dissolve the obtained solid with a small amount of ethanol, filter through a 0.2 μm filter membrane, and then prepare a high-efficiency liquid phase for further separation and purification by reverse phase, using C-8 bonded silica gel as the stationary phase, and 58% methanol aqueous solution as the For the mobile phase, set the flow rate to 20ml / min, set the wavelength of the UV detector to 310nm, guide the collection of the target eluent, recover the reagent to a small volume, place the crystals, filter out the crystals and heat them under reflux with methanol to dissolve them, let them cool down and cr...

Embodiment 2

[0024] Take 1Kg of Sophora flavescens, crush it, add 5L of 70% ethanol for ultrasonic extraction three times, combine the extracts, concentrate to obtain 71g of extract, add 800ml of sulfuric acid aqueous solution of pH5 to the extract for ultrasonic dispersion, remove the acid water layer by centrifugation, and repeat the acid water for solids Wash 3 times, dissolve the obtained solid with a small amount of ethanol, filter through a 0.45 μm filter membrane, and then use reverse phase to prepare high performance liquid phase for further separation and purification, with C-18 bonded silica gel as the stationary phase and 60% acetonitrile aqueous solution as the mobile phase Phase, set the flow rate to 30ml / min, set the wavelength of the UV detector to 310nm, guide the collection of the target eluent, recover the reagent to a small volume, place the crystal, filter out the crystal and heat it with methanol to reflux to dissolve, let it cool and crystallize 3 times , and the cryst...

Embodiment 3

[0026] Take 5Kg of Sophora flavescens, crush it, add 40L of 50% ethanol for ultrasonic extraction twice, combine the extracts, concentrate to obtain 286g of extract, add 2.4L of pH3 hydrochloric acid aqueous solution to the extract for ultrasonic dispersion, remove the acid water layer by centrifugation, and repeat the acid extraction of solids. Wash 3 times with water, dissolve the obtained solid with a small amount of ethanol, filter through a 0.3 μm filter membrane, and then use reverse phase to prepare high-efficiency liquid phase for further separation and purification, with C-18 bonded silica gel as the stationary phase and 62% methanol aqueous solution as the mobile phase Phase, set the flow rate to 60ml / min, set the wavelength of the UV detector to 310nm, guide the collection of the target eluent, recover the reagent to a small volume, place the crystal, filter out the crystal and heat it to reflux with methanol to dissolve, let it cool and crystallize twice , and the c...

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Abstract

The invention belongs to the field of separation of natural products, and provides a preparation method of trifolirhizin. The preparation method comprises the following steps of: performing methanol extraction; performing impurity removal with acid water to obtain total flavonoid; performing high performance liquid chromatography to purify; and finally thermally refluxing and crystallizing with methanol to obtain high-purity trifolirhizin. A product prepared by the preparation method has high purity and high quality.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, and in particular relates to a method for preparing pteroside from Sophora flavescens by using high-performance liquid phase preparative chromatography. Background technique: [0002] Sophora flavescens is the dried root of Sophora flavescens Ait., a perennial deciduous subshrub of the leguminous family Sophora genus. It has the effects of clearing heat and dampness, killing insects and diuresis, and can be used as bitter stomach invigorating agent, diuretic, anti-inflammatory drug, antidiarrheal drug and anthelmintic. [0003] The main functional components of Sophora flavescens are flavonoids and alkaloids. In recent years, there have been many studies on the flavonoids of Sophora flavescens, and relevant results have been obtained. Modern clinical research shows that the total flavonoids of Sophora flavescens has the functions of antibacterial and anti-inflammatory, slowing hear...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/065C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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