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A method for purifying troxerutin from troxerutin waste liquid powder

A waste liquid and wet method, applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc.

Active Publication Date: 2020-08-25
西安市美佳化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Purification of troxerutin by methanol recrystallization is simple and easy to operate, but it is only suitable for raw materials with high troxerutin content

Method used

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  • A method for purifying troxerutin from troxerutin waste liquid powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1, according to the sample amount of 2g troxerutin waste liquid powder / 100g silica gel, weigh 200-300 mesh silica gel (100g silica gel) and activate it at 100°C for 1 hour, then put the activated silica gel into the container, And add an appropriate amount of eluent, stir along a fixed direction, and when there are no air bubbles in the silica gel, put it into a silica gel chromatography column by wet method, the silica gel column is 3.5×30cm, and then use the eluent to balance the layer at a flow rate of 8mL / min Column analysis; wherein the eluent is: a mixture of acetone, ethyl acetate, water and glacial acetic acid, wherein the volume ratio of acetone, ethyl acetate, water and glacial acetic acid is: 10:10:3:1;

[0031] Step 2, sample loading: Dissolve 2g of troxerutin waste liquid powder in mobile phase and load the sample by wet method;

[0032] Step 3, elution: use the eluent to perform isocratic elution on the troxerutin waste liquid powder after wet loading...

Embodiment 2

[0039] Step 1, according to the loading amount of 2.5g troxerutin waste liquid powder / 100g silica gel, weigh 200-300 mesh silica gel (100g silica gel) and activate it at 101°C for 1.5h, then put the activated silica gel into the container Add an appropriate amount of eluent and stir in a fixed direction. When there are no air bubbles in the silica gel, put it into the silica gel chromatography column by wet method. The silica gel column is 3.5×30cm, and then use the eluent to Equilibrium chromatography column; eluent: a mixture of acetone, ethyl acetate, water and glacial acetic acid, wherein the volume ratio of acetone, ethyl acetate, water and glacial acetic acid is: 10.1:10.1:3:1;

[0040] Step 2, sample loading: 2.5g of troxerutin waste liquid powder was dissolved in mobile phase and then loaded by wet method;

[0041] Step 3, elution: use the eluent to perform isocratic elution on the troxerutin waste liquid powder after wet loading in step 2, the flow rate of the eluent ...

Embodiment 3

[0047] Step 1, according to the loading amount of 3g troxerutin waste liquid powder / 100g silica gel, weigh 200-300 mesh silica gel (100g silica gel) and activate it at 102°C for 2 hours, then put the activated silica gel into the container, And add an appropriate amount of eluent, stir along a fixed direction, and when there are no air bubbles in the silica gel, put it into a silica gel chromatography column by wet method, the silica gel column is 3.5×30cm, and then use the eluent to balance the layer at a flow rate of 8mL / min Column analysis; eluent: a mixture of acetone, ethyl acetate, water and glacial acetic acid, wherein the volume ratio of acetone, ethyl acetate, water and glacial acetic acid is: 10.2:10.15:3.1:1;

[0048] Step 2, sample loading: 3 g of troxerutin waste liquid powder was dissolved in mobile phase and then loaded by wet method;

[0049] Step 3, elution: use the eluent to perform isocratic elution on the troxerutin waste liquid powder after wet loading in ...

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Abstract

The invention discloses a method of purifying troxerutin from troxerutin wastewater powder. The method comprises the following steps: step one, column packaging: activating silica gel, performing silica gel wet column packaging, and then balancing the chromatographic column by using an eluant; step two, sample loading: dissolving troxerutin wastewater powder by the eluant, and performing wet sample loading; step three, elution: performing elution on the troxerutin wastewater powder after the wet sample loading in the step two, performing TLC analysis and detection, then collecting an elution liquid A containing troxerutin, and performing reduced pressure concentration to obtain crude troxerutin extractive; and step four: dissolving the crude troxerutin extractive obtained in the step three, performing membrane filtration, performing further separation purification by using semi-preparative high performance liquid chromatography, collecting an elution liquid B containing troxerutin, performing reduced pressure concentration and freeze drying to obtain tan troxerutin powder. In the method provided by the invention, a purification method combining silica gel column chromatography with semi-preparative high performance liquid chromatography is used to process the troxerutin wastewater powder to obtain the troxerutin with a concentration of 98%.

Description

technical field [0001] The invention relates to the technical field of raw material drug purification methods, in particular to a method for purifying troxerutin from troxerutin waste liquid powder. Background technique [0002] Troxerutin (Troxerutin), alias Toxerutin, trihydroxyethyl rutin, venoruton, vitamin P4, chemical name 3',4',7-tri[O-(2-hydroxyethyl) -5-hydroxyflavone-3]-rutin. Troxerutin is yellow or yellow-green powder, odorless, hygroscopic; easily soluble in water, slightly soluble in methanol, very slightly soluble in ethanol, insoluble in chloroform. Its molecular formula is C 33 h 42 o 19 , the molecular weight is 742.68, and the structural formula is as follows: [0003] [0004] Troxerutin is the main ingredient of Vebrarutong. Its pharmacological effects include inhibiting the aggregation of red blood cells and platelets, preventing thrombus formation, improving microcirculation, increasing the oxygen content in the blood, and promoting the format...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/06
CPCC07H1/06C07H17/07
Inventor 刘少静杨黎彬余丽丽李立姚琳陈卓
Owner 西安市美佳化工有限公司
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