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Preparation method and application of molecularly imprinted polymer

A molecular imprinting and polymer technology, applied in organic chemistry and other directions, can solve the problems of large solution concentration, complex preparation process and high cost, and achieve the effect of saving time, expanding the scope of application and simplifying the preparation process.

Inactive Publication Date: 2011-08-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solution concentration of template molecules used in the determination of the adsorption isotherm described in this experiment is obviously too high, and we cannot repeat the test experiment, so we have serious doubts about the credibility of the results
Another Chinese invention patent application 201010167614.0 proposes a method for preparing a core-shell structure composite nanometer surface molecularly imprinted polymer. The preparation process of this method is complicated and the cost is high, which is not conducive to large-scale preparation and application.

Method used

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  • Preparation method and application of molecularly imprinted polymer
  • Preparation method and application of molecularly imprinted polymer
  • Preparation method and application of molecularly imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 0.5mmol template molecule tanshinone IIA, 2.5mmol functional monomer methacrylic acid (MAA), 10mmol crosslinking agent ethylene glycol dimethacrylate (EDMA), 0.05g initiator azobisisobutyronitrile (AIBN) 1. Put 5mL porogen chloroform into a 50mL ground-mouthed round-bottom flask, and sonicate for 10min until uniformly mixed. After passing nitrogen gas in an ice bath for 10 minutes, seal it; place it in a constant temperature water bath at 60°C for polymerization for 24 hours to obtain a red rod-shaped polymer. The polymer was taken out, soaked in methanol, dried, and sieved. First use 2×100mL methanol to ultrasonically wash, filter with suction, then use 5×100mL1 methanol:acetic acid (V:V=9:1) mixed solution to ultrasonically wash, centrifuge, discard the upper washing solution, and then use 4×100mL methanol to ultrasonically clean Washing, suction filtration, repeated washing until no template molecule is detected under ultraviolet 270nm, and drying in a vacuum ...

Embodiment 2

[0030] Weigh 0.5mmol template molecule tanshinone IIA, 2.5mmol functional monomer 2-vinylpyridine (2-VP), 10mmol crosslinking agent trimethylolpropane trimethacrylate (TRIM), 0.05g initiator azobis Isobutyronitrile (AIBN), 5mL porogen dichloromethane, placed in a 50mL ground-mouth round bottom flask, sonicated for 10min until uniformly mixed. After passing nitrogen gas in an ice bath for 10 minutes, seal it; place it in a constant temperature water bath at 65°C for 8 hours to polymerize, and obtain a red rod-shaped polymer. The polymer was taken out, soaked in methanol, dried, and sieved. First use 2×100mL methanol to ultrasonically wash, filter with suction, then use 6×100mL methanol:acetic acid (V:V=9:1) mixed solution to ultrasonically wash, centrifuge, discard the upper washing solution, and then use 5×100mL methanol to ultrasonically clean Washing, suction filtration, and repeated washing until no template molecule is detected under ultraviolet light at 270 nm, and dryin...

Embodiment 3

[0032] Weigh 0.5mmol template molecule tanshinone IIA, 2.5mmol functional monomer acrylamide (AM), 10mmol crosslinking agent trimethylolpropane trimethacrylate (TRIM), 0.05g initiator azobisisobutyronitrile (AIBN ), 5mL porogen acetonitrile, placed in a 50mL ground-mouth round-bottom flask, ultrasonicated for 10min until uniformly mixed. After passing nitrogen gas in an ice bath for 10 minutes, seal it; place it in a constant temperature water bath at 60°C for 12 hours to polymerize to obtain a red rod-shaped polymer. The polymer was taken out, soaked in methanol, dried, and sieved. First use 2×100mL methanol to ultrasonically wash, filter with suction, then use 6×100mL methanol:acetic acid (V:V=8.5:1.5) mixed solution to ultrasonically wash, centrifuge, discard the upper washing solution, and then use 5×100mL methanol to ultrasonically clean Washing, suction filtration, repeated washing until no template molecule is detected under ultraviolet 270nm, and drying in a vacuum dr...

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Abstract

The invention provides a method for refining a molecularly imprinted polymer. The method comprises the following steps of: mixing tanshinone IIA serving as a template, a functional monomer, a cross-linking agent, an initiator and a pore-forming agent to prepare a homogeneous system; performing polymerization under the protection of nitrogen; grinding the prepared material into powder and sieving; and soaking, washing and eluting the powder with an alcohol solvent to obtain the molecularly imprinted polymer. The molecularly imprinted polymer prepared by the method represents high affinity and selectivity on the tanshinone IIA in an aqueous mobile phase, serves as a specific separating material and has a wide application prospect on separation, enrichment and purification of the tanshinone IIA in the Chinese medicament. In the method, materials are mixed in one step during synthesis; the preparation process is obviously simplified; time is saved; and an aqueous phase elution system is adopted, so that the application range is enlarged and the elution effect is obvious. The tanshinone IIA provided by the invention can serve as a solid phase extraction material to separate and purify the tanshinone IIA from a salvia miltiorrhiza bunge ethanol crude extract.

Description

technical field [0001] The invention belongs to the field of preparation of active ingredients of traditional Chinese medicines, and in particular relates to a method for preparing molecularly imprinted polymers and the application of the polymers in refining tanshinone IIA. Background technique [0002] Salvia miltiorrhiza has the effects of dispelling blood stasis and relieving pain, promoting blood circulation and promoting menstrual flow, clearing heart and eliminating troubles, and is a traditional Chinese medicine for treating cardiovascular and cerebrovascular diseases. The chemical composition of Danshen is mainly divided into two categories: fat-soluble components and water-soluble components. The fat-soluble components are mainly diterpenoids, such as tanshinone IIA, cryptotanshinone, and tanshinone I. Tanshinone compounds are fat-soluble main components, and their metabolites in vivo exhibit various pharmacological effects, and have potential therapeutic effects o...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F212/36C08F222/38C08F220/06C08F226/06C08F220/34C08F220/56C08F2/44C08J9/26C07D307/77
Inventor 王真真甘礼社周长新
Owner ZHEJIANG UNIV
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