Method for preparing core-shell structured composite nano surface molecular imprinting polymer of tanshinone compound

A molecular imprinting, compound technology, applied in the directions of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of low affinity efficiency, difficulty in removing template molecules, etc., and achieve binding rate and separation. High efficiency, improved mechanical strength and durability, high productivity

Inactive Publication Date: 2011-09-21
NANJING MEDICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this molecularly imprinted polymer is prepared in the form of bulk polymerization. A large number of imprinted binding points are located inside the material. It is very difficult to remove all the template molecules after synthesis. Usually, 5% of the template molecules remain, and the affinity efficiency after removal also very low
However, the application of molecular imprinting technology to separate and detect the metabolic components of Salvia miltiorrhiza in serum has not been reported yet.

Method used

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  • Method for preparing core-shell structured composite nano surface molecular imprinting polymer of tanshinone compound
  • Method for preparing core-shell structured composite nano surface molecular imprinting polymer of tanshinone compound
  • Method for preparing core-shell structured composite nano surface molecular imprinting polymer of tanshinone compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] At room temperature, add 2.8mL of concentrated ammonia water, 3.1mLTEOS and 1.3mL of distilled water into 100mL of absolute ethanol solution with high-speed magnetic stirring at a speed of 500rpm, and magnetically stir for 24 hours; repeatedly ultrasonically wash with absolute ethanol until neutral, centrifuge, and store at 40°C dried under vacuum to constant weight to obtain monodisperse NanoSiO 2 particles.

[0027] Weigh the prepared SiO 2 Ultrasonic disperse 0.5g particles in 50mL toluene solution, add 7.5mL MTPU, pass N under magnetic stirring 2 Deoxygenation, rotation speed is 500rpm, stirred and refluxed at 55°C for 24h to prepare NanoSiO 2 -MTPU, then ultrasonically washed with toluene and methanol, centrifuged to remove unreacted MTPU, dried in vacuum at 40°C for 12 hours, and set aside.

[0028] Take 0.1114g of the template molecule and 0.09mL of the functional monomer MAA dissolved in 25mL of acetonitrile solution, shake well, and let stand at 25°C for 4h ...

Embodiment 2

[0032] At room temperature, quickly add 12mL concentrated ammonia water, 3.6mL TEOS and 2.1mL distilled water into 100mL absolute ethanol solution with high-speed magnetic stirring at a speed of 1500rpm, and magnetically stir for 24 hours; repeatedly ultrasonically wash with absolute ethanol until neutral, centrifuge, and store at 40°C dried under vacuum to constant weight to obtain monodisperse NanoSiO 2 particles.

[0033] Weigh the prepared SiO 2 Ultrasonic dispersion of 0.5g of particles in 50mL of toluene solution, adding 12.5mL of MTPU, deoxygenation by passing nitrogen gas under magnetic stirring at 500rpm, stirring and reflux at 55°C for 24h, to prepare NanoSiO 2 -MTPU, then ultrasonically washed with toluene and methanol, centrifuged to remove unreacted MTPU, dried in vacuum at 40°C for 12 hours, and set aside.

[0034] Take 0.1114g of the template molecule and 0.11mL of the functional monomer MAA dissolved in 25mL of acetonitrile solution, shake well, and let stand...

Embodiment 3

[0038] At room temperature, quickly add 4.1mL concentrated ammonia water, 3.8mL TEOS and 1.7mL distilled water into 100mL absolute ethanol solution with high-speed magnetic stirring at a speed of 1000rpm, and magnetically stir for 24 hours; repeatedly ultrasonically wash with absolute ethanol until neutral, and centrifuge for 40 The monodisperse NanoSiO was prepared by vacuum drying at ℃ to constant weight. 2 particles.

[0039] Weigh the prepared SiO 2 Ultrasonic dispersion of 0.5g of particles in 50mL of toluene solution, adding 10mL of MTPU, nitrogen deoxygenation under magnetic stirring, rotation speed of 500rpm, stirring and reflux at 55°C for 24h, prepared NanoSiO 2 -MTPU, then ultrasonically washed with toluene and methanol, centrifuged to remove unreacted MTPU, dried in vacuum at 40°C for 12 hours, and set aside.

[0040] Take 0.1114g of the template molecule and 0.13mL of the functional monomer MAA in 25mL of acetonitrile solution, shake well, and let stand at 25°C ...

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Abstract

The invention relates to a method for preparing a core-shell structured composite nano surface molecular imprinting polymer of a tanshinone compound, which comprises preparation of a core monodisperse nano silicon dioxide particle. The method comprises the following preparation steps of: carrying out surface grafting modification on the prepared core monodisperse nano silicon dioxide particle, adding a template molecule and a functional monomer into 25mL of pore forming agent for mixing to prepare a preassembled solution and ultrasonically dispersing NanoSiO2-MTPU into the other 20mL of pore forming agent; then mixing the preassembled solution with the NanoSiO2-MTPU dispersed into the pore forming agent, adding a cross-linking agent and an initiating agent, stirring, importing nitrogen for removing oxygen and heating for triggering polymerization in the presence of the protection of the nitrogen; after the reaction is finished, centrifuging for removing supernatant, repeatedly and ultrasonically washing a product by a methanol-glacial acetic acid mixing solution till the template molecule can not be detected in the supernatant in an ultraviolet way; and then vacuum drying to constant weight and obtaining the core-shell structured composite nano surface molecular imprinting polymer of the tanshinone compound. The method can realize high selective separation, enrichment and detection on the tanshinone compound.

Description

1. Technical field [0001] The invention belongs to the technical field of molecularly imprinted polymers, and in particular relates to a preparation method of molecularly imprinted polymers with specific recognition for tanshinone compounds. 2. Background technology [0002] Salvia miltiorrhiza is the dry root and rhizome of Salva miltiorrhiza Bge., a plant of the Labiatae family. It has very significant effects of expanding coronary arteries, improving microcirculation, and protecting the heart. It is one of the most commonly used traditional Chinese medicines for promoting blood circulation and removing blood stasis. At present, Danshen and its preparations have been sold and used as medicines or food additives in more than a dozen countries around the world, and have been widely recognized worldwide. Since the 1930s, people have done a lot of research work on the chemical components and pharmacological effects of Danshen single herb and its compound. parts. At present, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F220/06C08F2/44C08J9/26B01J20/28B01J20/30B01J20/26B01J20/285
Inventor 陈立娜都述虎贾宪军刘利萍罗晶
Owner NANJING MEDICAL UNIV
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