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Nano superparamagnetic molecularly imprinted magnetic bead and preparation method and application thereof

A superparamagnetic and molecularly imprinted technology, applied in the field of chemical analysis and detection, can solve the problems of no molecularly imprinted magnetic beads, stability and separation efficiency, and achieve the effects of improving detection sensitivity, good dispersion stability, and reducing interference factors

Inactive Publication Date: 2020-10-16
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing molecularly imprinted magnetic beads have problems in terms of stability and separation efficiency, and there is no molecularly imprinted magnetic beads for sildenafil molecule

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The present embodiment belongs to the optimum selection of the present invention, and concrete steps are as follows:

[0033] (1) Polyacrylic acid modified superparamagnetic Fe 3 o 4 Preparation of nanoparticles: Under the protection of inert gas, inject 1.5mL of sodium hydroxide diethylene glycol solution with a mass concentration of 0.1g / mL into 30mL of anhydrous ferric chloride and polyacrylic acid with concentrations of 2M and 25M respectively , reacted at 200°C for 1.5h, and finally washed to obtain superparamagnetic Fe with a particle size of 70nm 3 o 4 Nanoparticles;

[0034] (2) Fe 3 o 4 @SiO 2 Preparation of nanoparticles: adding 3mL TEOS and 6mL ammonia water (28%) to 9mL mass concentration of 6g / L polyacrylic acid modified superparamagnetic Fe 3 o 4 Nanoparticles in anhydrous ethanol dispersion, reacted at 30°C for 3.5h, then centrifuged and washed 3 times with absolute ethanol as a dispersant, and then dried at 80°C for 12h to obtain Fe with a partic...

Embodiment 2

[0039] This embodiment is on the basis of embodiment 1, change Fe 3 o 4 @SiO 2 -The process of step (1) in the MIP preparation process, other preparation processes remain unchanged. Specifically, the concentration of sodium hydroxide diethylene glycol solution in step (1) was adjusted to 1 g / mL, and the concentrations of anhydrous ferric chloride and polyacrylic acid were increased to 4M and 45M respectively.

[0040] Gained Fe through the process of this embodiment 3 o 4 @SiO 2 -The size of MIP is 300nm, and it does not have superparamagnetic properties, and the particles are in agglomerated state. The efficiency of sildenafil molecular adsorption is low (1h, 30%), and a good separation and enrichment effect cannot be achieved.

Embodiment 3

[0042] This embodiment is on the basis of embodiment 1, change Fe 3 o 4 @SiO 2 -The process of step (2) in the MIP preparation process, other preparation processes remain unchanged. Specifically, the amount of TEOS was increased to 10 mL in step (2), and the reaction time was increased to 8 h.

[0043] Gained Fe through the process of this embodiment 3 o 4 @SiO 2 -MIP scale 100nm, SiO 2 The thickness of the shell layer has reached about 30nm, which greatly reduces the saturation magnetization (30emu / g) of the material. Although a good adsorption efficiency (2min, 90%) has been achieved during the molecular adsorption process of sildenafil, its magnetic Responsiveness is poor, separation effect is poor (40%), thus the expected sensitivity is not achieved in the later detection.

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Abstract

The invention belongs to the technical field of chemical analysis and detection, and particularly relates to a nano superparamagnetic molecularly imprinted magnetic bead and a preparation method and application thereof. The preparation method of the molecularly imprinted magnetic bead comprises three steps of preparation of a superparamagnetic nano material, coating modification of surface silicondioxide and preparation of surface molecularly imprinted modification. The molecularly imprinted magnetic bead for identifying sildenafil disclosed by the invention has a high-selectivity adsorptioneffect on sildenafil molecules; the adsorbent can be used for adsorption and enrichment of sildenafil molecules, has the advantages of large specific surface area, good dispersibility, large adsorption capacity, strong magnetic responsiveness and good stability, and is beneficial to improvement of the detection sensitivity of trace sildenafil molecules in food, drugs, health products and other products in combination with chromatography, electrochemistry and other detection technologies.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis and detection, and in particular relates to a nanometer superparamagnetic molecularly imprinted magnetic bead, a preparation method and an application. Background technique [0002] Sildenafil is a drug for the treatment of male sexual dysfunction. Improper use can cause adverse reactions such as headache, indigestion, and decreased ability to distinguish colors, and even death. Then, in order to improve the product effect and seek the maximum benefit of the product, criminals have illegally added sildenafil to food, medicine, health care products and other products in recent years. Although the amount added is very small, it has caused great harm to consumers. And because the added amount is small, the detection is difficult, and the harm of the product has great concealment. In recent years, many detection techniques have been used in the detection of trace sildenafil molecules in rel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30G01N1/28G01N1/38G01N1/40C08F222/14C08F220/04C08J9/28C08L35/02
CPCB01J20/06B01J20/103B01J20/268B01J20/28007B01J20/28009B01J20/28021C08J9/28C08J2335/02C08F222/102G01N1/28G01N1/38G01N1/40C08F220/04
Inventor 刘雪峰王子龙彭秀英董培智马学文芦冬涛
Owner SHANXI UNIV
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