A polymer monolithic column for on-line enrichment and purification of ursolic acid and a method for on-line enrichment and purification of ursolic acid

A technology of ursolic acid and polymer, which is applied in the field of preparation of separation materials, can solve the problems of large amount of solvent, long sample pretreatment time, small specific surface area, etc., and achieves shortened pretreatment time, good purification effect and simple preparation method Effect

Active Publication Date: 2022-03-04
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Monolithic columns can be used as solid-phase extraction adsorbents for the extraction, separation and detection of trace targets in food, environmental samples, or biological samples, but they also have disadvantages such as small specific surface area, poor adsorption performance, uneven structure, and poor repeatability. How to make a monolithic column with uniform structure, good selectivity and large adsorption capacity is of great significance.
[0005] In order to facilitate sample pretreatment and analysis, solid-phase extraction is usually used in conjunction with analytical instruments. In the prior art, offline extraction is often used to enrich ursolic acid and then enter the analytical instrument. The amount of solvent used is large, and only a small part of the sample can be injected. Analytical instrument, the adsorption capacity needs to be improved, the operation steps are cumbersome, the sample pretreatment time is long and the loss is large, the recovery rate is low, the precision and reproducibility are poor

Method used

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  • A polymer monolithic column for on-line enrichment and purification of ursolic acid and a method for on-line enrichment and purification of ursolic acid
  • A polymer monolithic column for on-line enrichment and purification of ursolic acid and a method for on-line enrichment and purification of ursolic acid
  • A polymer monolithic column for on-line enrichment and purification of ursolic acid and a method for on-line enrichment and purification of ursolic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 4.3g pyromellitic acid and 2.3g ZrCl 4 Dissolve in ultrapure water at room temperature, reflux for 24 hours, wash the obtained white jelly, dissolve in ultrapure water and continue to reflux for 16 hours, centrifuge, wash, and dry the obtained solid to obtain a carboxyl-containing MOFs material. Disperse 1 mol of MOFs material with carboxyl groups and 1 mol of KH-570 in toluene and reflux for 8 hours to obtain derivatized MOFs material with carbon-carbon double bond, that is, functionalized MOFs material.

[0050] Precisely weigh 0.003g of benzoyl peroxide, 0.05g of N-isopropylacrylamide, and 0.002g of derivatized MOFs with carbon-carbon double bonds into a centrifuge tube, and immediately add 0.8mL of n-propanol, 0.8mL Polyethylene glycol 400 and 0.35mL ethylene glycol dimethacrylate, vortex and ultrasonic for 1h to disperse until the mixture is uniform, add N,N-dimethylaniline, mix quickly, put into a stainless steel column, After reacting for 3.5 hours in a water ba...

Embodiment 2

[0054] Under the same conditions as in Example 1, put 0.003g of benzoyl peroxide into a centrifuge tube, add 0.05g of N-isopropylacrylamide, 0.8mL of n-propanol, 0.8mL of polyethylene glycol 400 and 0.35mL of ethyl alcohol Diol dimethacrylate, vortex and ultrasonic for 1h to disperse until the mixture is uniform, add N,N-dimethylaniline, mix quickly, put it into a stainless steel column, and react in a water bath at 30°C for 3.5h. That is, a polymer monolithic column without MOFs material is obtained.

[0055] The microscopic morphology of the monolithic column prepared above was observed with a scanning electron microscope, and the obtained results are as follows: Figure 4 . The nitrogen adsorption-desorption isotherm of the monolithic column was measured with a specific surface area measuring instrument as image 3 As shown in the curve b, its specific surface area is 35.0921m 2 / g.

Embodiment 3

[0057] Under the same conditions as in Example 1, put 0.003g of benzoyl peroxide and 0.002g of derivatized MOFs with carbon-carbon double bonds into a centrifuge tube, add 0.05g of N-isopropylacrylamide, 0.25mL of ethylene diacetate Alcohol dimethacrylate, 0.8mL n-propanol, 0.8mL polyethylene glycol 400, vortex, ultrasonic 1h to disperse, until the mixture is uniform, add N,N-dimethylaniline, mix quickly, put into In the stainless steel column, after 3.5 hours of constant temperature reaction in a water bath at 30°C, the polymer monolithic column was obtained. The microscopic morphology of the monolithic column prepared above was observed with a scanning electron microscope, and the obtained results are as follows: Figure 5 .

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Abstract

The invention provides a polymer monolithic column for on-line enrichment and purification of ursolic acid and a method for on-line enrichment and purification of ursolic acid. The polymer monolithic column is an integral porous material, which adopts derivatization with The metal-organic framework material with carbon-carbon double bond, N-isopropylacrylamide and ethylene glycol dimethacrylate are prepared by redox polymerization. The preparation method of the present invention is simple, and the obtained polymer monolithic column has excellent performances such as specific surface area, pore structure, and adsorption property, and its interaction force with ursolic acid is strong, and ursolic acid can be effectively separated and enriched, and the ursolic acid in actual samples can be effectively separated and enriched. Ursolic acid has good purification effect, good repeatability, high recovery rate, and simplifies the operation steps of sample pretreatment, greatly reduces the pretreatment time of samples, and is economical and practical.

Description

technical field [0001] The invention relates to the field of separation material preparation, in particular to a polymer monolithic column 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 is a pentacyclic triterpene that belongs to the group of C30 isoprenoids. Studies have shown that ursolic acid has a variety of pharmacological effects, such as anti-inflammation, anti-oxidation, anti-cancer, cardioprotection, neuroprotection, liver protection and immune regulation, and has high activity and low toxicity. Therefore, ursolic acid has been More and more attention has been paid to it, and it has become one of the current research hotspots. [0003] Ursolic acid is widely found in herbs, leaves, flowers and fruits. For example, rosemary contains diterpene phenols, flavonoids, triterpenoids and essential oils. Among them, oleanolic acid and ursolic acid are I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08
CPCG01N30/08
Inventor 刘海燕庞晓雅白立改闫宏远
Owner HEBEI UNIVERSITY
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