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Method for preparing estradiol molecularly imprinted magnetic microsphere

A technology of molecular imprinting and magnetic microspheres, applied in the fields of materials science and engineering and environmental science, can solve the problems that restrict the preparation and application of MIPs, and achieve the effect of improving the recognition rate, regular morphology and good monodispersity.

Active Publication Date: 2014-11-12
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, how to simplify the preparation steps to speed up the experimental process, how to improve the polymerization yield and product stability, how to further increase the imprinting capacity, how to improve the elution and separation efficiency of molecularly imprinted materials, etc., still restrict the preparation and application of MIPs.

Method used

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  • Method for preparing estradiol molecularly imprinted magnetic microsphere
  • Method for preparing estradiol molecularly imprinted magnetic microsphere
  • Method for preparing estradiol molecularly imprinted magnetic microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] a.Fe 3 o 4 Magnetic material preparation: Accurately weigh 1.35g of FeCl 3 6H 2 O is placed in a 100mL small beaker, and 40mL of ethylene glycol is added. After stirring evenly, add 2.17g of anhydrous sodium acetate, sonicate for 30 minutes, add 3g of polyethylene glycol 4000 after the dissolution is complete, and stir in a water bath at 60°C until dissolved. Then the solution was transferred to a 50mL reaction kettle, placed in an oven at 200°C for 10h, and taken out after natural cooling. The product was washed 5 times with absolute ethanol and deionized water, and then placed in a fume hood to dry naturally. The resulting pure black Fe 3 o 4 The product is sealed and stored.

[0039] b.Fe 3 o 4 SiO 2 Preparation of core layer material: 2.0g of the above Fe 3 o 4 Disperse in 60mL ethanol and 10mL deionized water, put in a 250mL single-necked round bottom flask, ultrasonically treat for 15min, then add 1mL ammonia water drop by drop while stirring mechanical...

Embodiment 2

[0045] At room temperature, weigh 0.5 mg of 17β-estradiol standard substance, dissolve it with acetonitrile and dilute it into a 100 mL volumetric flask to obtain a 5 mg / L 17β-estradiol solution, which is stored for future use. Put 20 mg of magnetic molecularly imprinted polymers (M-MIPs) into 2 mL of acetonitrile solution containing the above 5 mg / L 17β-estradiol, and after 3 h of shaking adsorption at room temperature, use a magnet to adsorb on one side of the vial for 10 min , the imprinted microspheres can be adsorbed to one side, and a clear solution can be obtained again. Such as image 3 As shown in the inset, the microspheres have a strong adsorption capacity for 17β-estradiol, and the separation process is fast and simple. see image 3 The hysteresis loop indicates that the M-MIPs have a high magnetic intensity.

Embodiment 3

[0047] At room temperature, weigh 20 mg of 17-β-estradiol standard substance, dissolve it with acetonitrile and dilute it into a 100-mL volumetric flask to obtain a 200 mg / L 17-β-estradiol solution, which is stored for future use. Then dilute to 1, 10, 20, 40, 60, 80, 100mg / L with acetonitrile solution, take 2mL respectively and place them in seven 10mL test tubes with ground mouth and stoppers, and add 20mg of magnetic molecularly imprinted polymer ( M-MIPs). As a comparison, 20 mg of magnetic non-imprinted polymers (M-NIPs) were added to the other 7 vials. At room temperature, shake and adsorb for 12 hours, then centrifuge the mixture and filter it with a 0.45 μm microporous membrane. The concentration of 17β-estradiol in the supernatant is determined by HPLC-UV. The original concentration of 17β-estradiol is reduced The remaining concentration in the supernatant was the adsorption amount of the imprinted microspheres, and each experiment was measured 3 times in parallel. ...

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Abstract

The invention belongs to the field of materials science and engineering and environmental sciences, and particularly relates to a method for preparing an estradiol molecularly imprinted magnetic microsphere in a controllable living polymerization potful compositing mode. According to the method, a reversible addition-fracture chain transfer controllable living free radical polymerization and precipitation polymerization potful compositing mode is adopted, molecularly imprint with 17 beta estradiol as a template and a sensitive material are combined, and then the estradiol molecularly imprinted magnetic microsphere is obtained. The microsphere obtained through the method is high in adsorption capacity for 17 beta estradiol, has the high-speed dynamic character and the superior recognizing and selecting performance, is separated conveniently and quickly under the action of an applied magnetic field, and is good in reusing performance. According to the method, the character of reversible addition-fracture chain transfer controllable living polymerization is utilized fully, step-by-step feeding potful operation is adopted to prepare the core-shell structure printed microsphere, the surface printing process is effectively simplified, the experimental period is shortened, the recognizing speed is greatly improved, and the printing capacity is increased.

Description

technical field [0001] The invention belongs to the fields of material science and engineering and environmental science, and specifically relates to a method for preparing estradiol molecularly imprinted magnetic microspheres by using controllable active polymerization and one-pot synthesis. Background technique [0002] 17β-estradiol is one of the most important phenolic environmental endocrine disrupting hormones, and its benzoate is one of the reference substances for determining the international unit of sex hormone potency. In addition to regulating and maintaining the normal balance of the human endocrine system, 17β-estradiol also plays an important role in maintaining bone health and protecting the cardiovascular system, and can affect people's behavior and mood. However, more and more evidence shows that a slight excess of 17β-estradiol can cause adverse physiological reactions, damage the endocrine system, induce cancer and even cause death. The low dose and high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/36C08F220/56C08F2/44C08K3/22C08K3/36C08J9/28G01N30/08
Inventor 李金花陈令新董瑞晨
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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