Preparation method and application of phloroglucinol molecularly imprinted polymers in plants

A molecular imprinting and phloroglucinol technology, applied in the separation/purification of carbonyl compounds, separation methods, solid adsorbent liquid separation, etc., can solve the problems of high time and cost, large amount of organic solvent, complicated separation process, etc. , to achieve the effect of simple operation, high separation efficiency and recovery rate, and large adsorption capacity

Inactive Publication Date: 2012-07-18
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All of the above methods can obtain the target compound with a certain purity, but the separation process i...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of molecularly imprinted polymers of phloroglucinol compounds

[0023] Weigh 6g of polyvinyl alcohol 400 into 150mL of double distilled water, dissolve in hot water at 90°C-95°C, cool to room temperature, and then transfer to a 250mL three-necked flask. Accurately take 0.5mmol of the template molecule (hyperforin) and 2mmol of the functional monomer methacrylic acid, dissolve in 150mL of acetone, and after fully dissolved, sonicate for 5min, and then place it in a refrigerator at 4°C for 24h to form a stable complex. Pre-polymerization; then add 10 mmol of trimethylolpropane trimethacrylate as a cross-linking agent, 0.4 mmol of benzoyl peroxide and N, N-dimethylaniline as initiators, and slowly Drop it into the above-mentioned three-necked flask with a heating temperature of 20°C under stirring at 400 rpm, and initiate polymerization for 18 hours to form a milky white microsuspension emulsion, that is, imprinted polymer microspheres; the obtained imprint...

Embodiment 2

[0034] (1) Preparation of molecularly imprinted polymers of phloroglucinol compounds

[0035] The basic process of preparation is the same as in Example 1, the concentration of polyvinyl alcohol 400 used is 6%, the amount of porogen used is 200mL, the functional monomer is acrylamide 3mmol, and the crosslinking agent trimethylolpropane trimethacrylate is 15mmol , the initiators benzoyl peroxide and N, N-dimethylaniline are 0.6 mmol each, the polymerization initiation temperature is 25° C., the polymerization time is 12 hours, and the elution time of the polymer Soxhlet extraction is 18 hours.

[0036] (2) Characterization of molecularly imprinted polymers of phloroglucinol compounds

[0037] The characterization method is the same as in Example 1, and the results show that there are two types of adsorption sites in the template molecularly imprinted polymer, one is a highly selective binding site, and the other is a low-selective binding site (its K D1 =4.2×10 -2 mu mol / L, ...

Embodiment 3

[0044] (1) Preparation of molecularly imprinted polymers of phloroglucinol compounds

[0045] The basic process of preparation is the same as in Example 1, the concentration of polyvinyl alcohol 400 used is 5%, the amount of porogen used is 100mL, the functional monomer is methacrylate 4mmol, and the crosslinking agent trimethylolpropane trimethacrylic acid 20 mmol of ester, 0.8 mmol of benzoyl peroxide initiator and 0.8 mmol of N,N-dimethylaniline each, polymerization initiation temperature of 18°C, polymerization time of 24 hours, polymer Soxhlet extraction and elution time of 12 hours.

[0046] (2) Characterization of molecularly imprinted polymers of phloroglucinol compounds

[0047] The characterization method is the same as in Example 1, and the results show that there are two types of adsorption sites in the template molecularly imprinted polymer, one is a highly selective binding site, and the other is a low-selective binding site (its K D1 =3.7×10 -2 mu mol / L, Q m...

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PUM

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Abstract

The invention relates to a preparation method and application of phloroglucinol molecularly imprinted polymers in plants. The method comprises the following steps of: mixing template molecules, a functional monomer and a cross-linking agent in a molar ratio of 1:(3-6):(15-30), and adding benzoyl peroxide and N,N-dimethylaniline which serve as redox initiators; dripping the mixture into a 3 to 8 percent polyvinyl alcohol 400 aqueous solution with stirring at the temperature of between 10 and 30 DEG C to obtain polymer microspheres; bleaching the polymer microspheres, sieving, eluting, drying and the like, and filling in a glass chromatographic column by a wet method; and moistening the polymer microspheres by using methanol and acetone sequentially to obtain a molecularly imprinted chromatographic column, so that the molecularly imprinted chromatographic column is used for the preferential adsorption and efficient enrichment of phloroglucinol substances such as hyperforin, adhyperforinand the like. Compared with the conventional chromatographic column, the prepared chromatographic column has the characteristics that the column is high in specificity, easy and convenient to prepareand low in cost, required instruments and reaction conditions are easy to implement, and the like.

Description

technical field [0001] The invention relates to the technical field of chemical separation, in particular to the preparation of phloroglucinol molecularly imprinted polymers and the use of the polymers as column chromatography fillers for the separation and purification of hypericin and hyperforin in plants . Background technique [0002] Phloroglucinol substances widely exist in plants, which have pharmacological activities such as antidepressant, antibacterial, antitumor, anti-Alzheimer's disease, and promotion of learning and memory. Oxygen is very sensitive, and it can be completely oxidized after being stored at room temperature for a few days. In Hypericum perforatum, such substances are mainly hyperforin and hyperforin. The content of the former in the whole plant is 2%-4.5%, and the content of the latter is only 0.2%-1.9%. The structures of the two are very similar, and hyperforin has only one more methyl group than hyperforin, and has similar pharmacological activ...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/30B01D15/22C08F222/14C08F220/06C08F220/56C08F226/06C08F220/18C08J9/28C08J9/26C07C49/798C07C45/79
Inventor 李兆周李道敏侯玉泽杜琳徐航张敏刘世磊李志康李文荣
Owner HENAN UNIV OF SCI & TECH
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