Polymer continuous bed and method for online ursolic acid enrichment and purification

A technology of ursolic acid and polymers, which is applied in the field of separation material preparation, can solve the problems of cumbersome operation steps, increased adsorption capacity, large amount of solvent, etc., and achieve the effect of simplifying operation steps, reducing pretreatment time, and realizing green chemistry

Active Publication Date: 2019-10-25
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Solid-phase extraction is a commonly used sample pretreatment technology at present. In the prior art, offline extraction is often used to enrich ursolic acid. The amount of solvent is large, and only a small part of the sample can be injected into the analysis instrument. The adsorption capacity needs to be improved. The operation steps cumbersome, low recovery rate

Method used

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  • Polymer continuous bed and method for online ursolic acid enrichment and purification
  • Polymer continuous bed and method for online ursolic acid enrichment and purification
  • Polymer continuous bed and method for online ursolic acid enrichment and purification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Dissolve 0.2 g of hydroxylated multi-walled carbon nanotubes and 0.2 g of γ-methacryloxypropyltrimethoxysilane in 30 mL of 95% ethanol, heat at 60 °C for 6 h, and centrifuge to obtain silanized Double bonded multi-walled carbon nanotubes.

[0042] Precisely weigh 0.03g of benzoyl peroxide and 3.0mg of silanized multi-walled carbon nanotubes with double bonds into a centrifuge tube, add 0.35mL of styrene, 0.48mL of ethylene glycol dimethacrylate , 0.70mL n-butanol and 0.40mL isopropanol, vortex and sonicate for 30 minutes to disperse the solids in the mixture until the mixture is uniform, add N,N-dimethylaniline, mix quickly, put it into the chromatographic column tube, 30 After reacting in a water bath at ℃ for 3.0 h, a continuous bed of functionalized carbon nanotube polymer is obtained.

[0043] Adopt scanning electron microscope to observe the microscopic shape of the continuous bed that above-mentioned preparation obtains, the obtained result is as follows figure 1 ...

Embodiment 2

[0045] Under the same conditions as in Example 1, put 0.03g of benzoyl peroxide into a centrifuge tube, add 0.35mL of styrene, 0.48mL of ethylene glycol dimethacrylate, 0.70mL of n-butanol, and 0.40mL of isopropanol , use vortex to dissolve the solid in the mixture, disperse by ultrasonication for 30min until the mixture is uniform, add N,N-dimethylaniline, mix quickly, put it into the chromatographic column tube, and react in a 30℃ water bath for 3.0h, That is, a continuous bed of polymer without adding carbon nanotubes is obtained.

[0046] Observing the microscopic morphology of the continuous bed prepared above with a scanning electron microscope, the obtained results are as follows figure 2 . The nitrogen adsorption-desorption isotherm of this continuous bed is measured with a specific surface area measuring instrument as image 3 As shown, its specific surface area is 12.7505 m 2 / g.

Embodiment 3

[0048] Under the same conditions as in Example 1, put 0.03g benzoyl peroxide and 3.0mg silanized multi-walled carbon nanotubes with double bonds into a centrifuge tube, add 0.35mL styrene, 0.36mL ethylene glycol di Methacrylate, 0.70mL n-butanol, 0.40mL isopropanol, vortex and ultrasonic 30min to disperse the solid in the mixture until the mixture is uniform, add N,N-dimethylaniline, mix quickly, put In the chromatographic column tube, after 3.0 hours of constant temperature reaction in a water bath at 30°C, a continuous polymer bed is obtained. Observing the microscopic morphology of the continuous bed prepared above with a scanning electron microscope, the obtained results are as follows Figure 4 .

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Abstract

The invention provides a polymer continuous bed and method for online ursolic acid enrichment and purification. The polymer continuous bed of a whole porous material is prepared from multi-wall carbonnanotubes with double bonds after silylanization, styrene and ethylene glycol dimethacrylate by redox polymerization. The preparation method is simple, the polymer continuous bed for online ursolic acid enrichment and purification is high in specific surface area and excellent in porous structure, the active force between the polymer continuous bed and ursolic acid is increased, the ursolic acidcan be enriched online effectively, the adsorption quantity is large, the detection limit is low, the precision, sensitivity and accuracy of analysis and detection are improved, the recovery rate is high, operation steps as sample pretreatment are simplified, pretreatment time of samples is greatly reduced, and further the method is economic, practical and facilities green chemistry.

Description

technical field [0001] The invention relates to the field of separation material preparation, in particular to a polymer continuous bed for on-line enrichment and purification of ursolic acid and a method for on-line enrichment and purification of ursolic acid. Background technique [0002] Ursolic acid (Ursolic acid, UA), also known as ursolic acid, ursolic acid, is a pentacyclic triterpene saponin compound, and is a functional component of many natural products. As a pharmaceutical raw material with practical value, it is becoming more and more received the attention of the scientific community. Studies in recent years have shown that ursolic acid has various pharmacological effects. It is active against Gram-positive bacteria, Gram-negative bacteria, and yeasts. It also has calming, anti-hepatitis, antibacterial, anti-diabetic, and anti-viral properties. , reducing blood sugar, anti-cancer and other biological effects, among which the anti-tumor activity is particularly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
CPCG01N30/08
Inventor 刘海燕于欢白立改闫宏远
Owner HEBEI UNIVERSITY
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