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18beta-glycyrrhetinic acid molecularly imprinted polymer with metal ions as bridging agent and monolithic column

A glycyrrhetic acid, molecular imprinting technology, applied in the direction of ion exchange, steroids, ion exchange regeneration, etc., can solve the problems of low selectivity, high price, unstable properties, etc.

Inactive Publication Date: 2016-04-20
TIANJIN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many commercial adsorbents in solid phase extraction often co-extract for samples with complex components due to their low selectivity.
For highly selective SPE materials, this phenomenon can be avoided, but the price is too expensive and the properties are not stable

Method used

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  • 18beta-glycyrrhetinic acid molecularly imprinted polymer with metal ions as bridging agent and monolithic column
  • 18beta-glycyrrhetinic acid molecularly imprinted polymer with metal ions as bridging agent and monolithic column
  • 18beta-glycyrrhetinic acid molecularly imprinted polymer with metal ions as bridging agent and monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of molecularly imprinted monolithic columns using metal ions as bridging agents and 18β-glycyrrhetinic acid without metal ions as templates and comparison of their imprinting factors. Specific steps are as follows:

[0032] Preparation of 18β-glycyrrhetinic acid imprinted monolithic column by in situ polymerization:

[0033] a. The mass percent template 18β-glycyrrhetinic acid 3.09%, bridging agent cobalt acetate 1.64%, functional monomer 4-vinylpyridine 2.76%, initiator azobisisobutyronitrile 0.29%, crosslinking agent dimethacrylic acid Ethylene glycol ester 26.04%, dissolved in porogen 1-butyl-3-methylimidazolium tetrafluoroborate 43.59%, N,N-dimethylformamide 3.32%, dimethyl sulfoxide 19.27% In the mixed porogen solution; ultrasonically dissolved for 30min to dissolve and clarify, then pass nitrogen gas to remove the oxygen in the pre-polymerization mixture, and then inject the pre-polymerization mixture into a stainless steel column (100×4.6mmI.D.) , sea...

Embodiment 2

[0041] In order to characterize the morphological characteristics of 18β-glycyrrhetinic acid molecularly imprinted polymers with metal ions as bridging agents, 18β-glycyrrhetinic acid molecularly imprinted polymers MIP and 18β-glycyrrhetinic acid-free non-molecularly imprinted polymers NIP were prepared. And nitrogen adsorption-desorption analysis was carried out on the two polymers, the specific operation steps are as follows:

[0042] a. Preparation of polymer: dry the prepared polymer in the same way as above (Example 1), and grind it finely in a mortar.

[0043] b. Nitrogen adsorption test: put the ground 18β-glycyrrhetinic acid molecularly imprinted polymer MIP and 18β-glycyrrhetinic acid-free non-molecularly imprinted polymer NIP at 60oC for vacuum degassing (10 ?3 Torr) for 4 hours, take the dried particles and place them in the ASAP-2020 particle surface area and porosity analyzer, and process the obtained data to obtain the nitrogen adsorption-desorption isotherm and ...

Embodiment 3

[0046] In the process of solid-phase extraction, the adsorption of the target compound must go through four steps: adsorbent activation, sample loading, rinsing, and elution, among which rinsing is the most important. The purpose of rinsing is to convert non-specific adsorption of target molecules into specific adsorption, while washing away impurities while retaining target molecules. The selection principle of the eluting solvent is to retain the target molecule and to elute the impurity molecule. The present invention screens the washing solvent, and the concrete steps are as follows:

[0047] a. Preparation of polymer: Dry the prepared polymer in the same way as above (Example 1), grind it finely in a mortar, and sieve (74 μm).

[0048] b. Washing process: Pack 1g of the polymer in step a into a 3mL solid-phase extraction column. After the SPE (SolidPhaseExtraction) column is activated and 2mg of the crude extract is loaded, the washing operation is performed. The elutin...

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Abstract

The invention relates to an 18beta-glycyrrhetinic acid molecularly imprinted polymer with metal ions as a bridging agent and a monolithic column. The polymer is used as an adsorbing agent for solid phase extraction and separation of glycyrrhetinic acid epimers. The polymer is prepared from 1.55-4.12% of 18beta-glycyrrhetinic acid, 0.82-2.18% of cobaltous acetate, 2.73-2.80% of 4-vinyl pyridine, 0.26-0.32% of azodiisobutyronitrile, 15.63-31.25% of ethylene glycol dimethacrylate, 43.28-43.80% of 1-butyl-3-methylimidazolium tetrafluoroborate, 3.18-3.59% of N,N-dimethylformamide and 18.47-20.01% of dimethyl sulfoxide. Compared with an imprinted polymer with no metal ion, the imprinting factor of the polymer synthesized through the method is improved by about 3 times, and the polymer is dried, ground and screened (74 micrometers) to be used as an adsorbing agent to be placed into an SPE column for carrying out separation and enrichment on 18beta-glycyrrhetinic acid in glycyrrhetinic acid crude extract. The recovery rate of the obtained sample is 91.1%, and the purity of the obtained sample is 93.8%. Accordingly, the polymer can be used for separation, purification and enrichment of the glycyrrhetinic acid crude extract.

Description

technical field [0001] The invention relates to a 18β-glycyrrhetinic acid molecularly imprinted polymer and a monolithic column with metal ions as bridging agents. Background technique [0002] Licorice is a traditional Chinese herbal medicine with a sweet and flat taste. The main active ingredient in licorice is glycyrrhizic acid, but due to the different configuration of the 18-position chiral carbon atom, a pair of epimers 18α-glycyrrhizic acid and 18β-glycyrrhizic acid are produced, and after acid hydrolysis, 18α - Glycyrrhetinic acid and 18β-glycyrrhetinic acid. β-glycyrrhetinic acid is stronger than β-glycyrrhizic acid in terms of anti-virus. In addition, Sun Haoyang et al [Sun Haoyang, Li Qing, Chen Wei, et al. Pharmacokinetic study of glycyrrhetinic acid epimers in rats after single administration and combined administration [J]. Acta Pharmaceutica Sinica, 2012.] The pharmacokinetic study of glycyrrhetinic acid epimers in rats proves that the resolution of glycyrr...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F226/06C08J9/28C08J9/26C08K5/098B01J20/26B01J20/30B01D15/08C07J63/00
CPCB01D15/08B01J20/268B01J2220/4812B01J2220/58C07J63/008C08F222/1006C08F222/102C08J9/26C08J9/28C08J2201/0422C08J2335/02C08K5/098C08F226/06
Inventor 刘照胜李秀媛黄艳萍
Owner TIANJIN MEDICAL UNIV
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