Preparation method of chicoric acid imprinted monolithic column

Abstract

The invention relates to a preparation method of a chicoric acid imprinted monolithic column. The method comprises the following steps: adopting chicoric acid as a template, adding zinc acetate or cobalt acetate, using N,N-dimethyl formamide, dimethyl sulfoxide and 1-butyl-3-methylimidazolium tetrafluoroborate as a pore-foaming agent, then adding a functional monomer, a cross-linking agent or an initiator, then ultrasonically dissolving to remove dissolved oxygen, initiating the reaction, and finally obtaining the chicoric acid imprinted monolithic column with selectivity. By adopting the preparation method, the consumption of templates is less, and the imprint cost of the chicoric acid is greatly reduced. The chicoric acid imprinted monolithic column and a blank reference column are successfully synthesized in a stainless steel column tube, and the chromatographic performance optimization is carried out. Experiment results prove that imprinting factors are up to 24.81. The method is simple in preparation; and the macromolecular polymer is good in durability, and a cost-saving method is provided for the separation and purification of chicoric acid (the purity is higher than 98.5 percent).

Description

technical field [0001] The invention relates to a preparation method of a cichoric imprinted monolithic column. The imprinted polymer exhibits good selectivity for cichoric acid and can be used for the separation and purification of cichoric acid. Background technique [0002] Chichoric acid is one of the important immune active ingredients in chicory stems and leaves. In recent years, pharmacological studies have shown that cichoric acid can enhance immune function and anti-inflammatory effects, and can inhibit hyaluronidase and protect collagen from degradation. The impact of free radicals also has the effect of inhibiting HIV1 and HIV2 integrase and promoting the release of insulin. Therefore, cichoric acid has great medicinal value, and there is a large demand for cichoric acid in the market. [0003] At present, the traditional methods for extracting, separating, and preparing and purifying cichoric acid mainly include: supercritical CO 2 Extraction method, macroporous...

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Problems solved by technology

CN102060706A has reported that by supercritical CO 2 The extraction method extracts Echinacea purpurea with ethanol, then adds salt to disperse, alkalizes, elutes with anion exchange resin and cationic resin column, and the eluate is concentrated and dried to obtain cichoric acid. Although this method can obtain chicory with higher purity Sour, but cumbersome to operate

CN103641716A has reported that Echinacea purpurea obtains cichoric acid with a purity of 22% after processes such as ultrasonic extraction, vacuum decompression concentration, macroporous resin loading, deionized water rinsing, eluting, vacuum decompression concentration, etc., and what is obtained is only cichoric acid crude Body matter, unable to meet the requirements for medicinal use

CN101148410A has reported to obtain the larger cichoric acid of purity through ethanol extraction, macroporous resin adsorption elution, high-speed countercurrent chromatography purification, but process is complicated

[0005] However, the special structure of the cichoric acid molecule causes the molecule to form intramolecular hydrogen bonds. This effect competes with the interaction between the template molecule and the functional monomer, which often weakens the recognition performance of the prepared molecularly imprinted polymer and reduces its The effect of practical application

For example, Saad et al. use chicoric acid (CA) as a template molecule in "Preparation and application of molecularly imprinted polymer for isolation of chicoric acid from Chicorium intybusL..medicinal plant" (Analytica Chimica Acta.2015,877:80-89.), 4-vinylpyridine (4-VP) is a functional monomer, ethylene glycol dimethacrylate (EDMA) is a crosslinking agent, and the molar ratio of the template molecule, functional monomer and crosslinking agent is 1:4: 20. Using bulk and precipitation polymerization, CA molecularly imprinted polymers were synthesized, and cichoric acid was selectively separated from cichoric analogues, but pure cichoric acid was not obtained from the bold

Therefore, the synthesis of highly selective cichoric acid-imprinted polymers is an important challenge in the separation of real samples.

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