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Preparation method of molecularly imprinted polymer on nano-silica gel surfaces of sulfonylurea herbicides

A nano-silica gel and molecular imprinting technology, applied in chemical instruments and methods, other chemical processes, etc., can solve problems such as unsatisfactory polymer affinity efficiency and difficult removal, achieve efficient and rapid separation and enrichment, improve efficiency, Effects that are easy to chemically modify and design

Inactive Publication Date: 2010-06-30
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis of these molecularly imprinted polymers is prepared by bulk polymerization. Although the prepared materials are pulverized, there are still many template molecules inside the materials, which are difficult to remove when eluted; When , it is difficult for the template molecule to reach the internal binding site, so the affinity efficiency of the polymer is not ideal

Method used

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  • Preparation method of molecularly imprinted polymer on nano-silica gel surfaces of sulfonylurea herbicides
  • Preparation method of molecularly imprinted polymer on nano-silica gel surfaces of sulfonylurea herbicides
  • Preparation method of molecularly imprinted polymer on nano-silica gel surfaces of sulfonylurea herbicides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1. Preparation of SiO 2 small ball

[0032] Mix 50mL of absolute ethanol and 9mL of concentrated ammonia water to obtain solution A, and stir magnetically at high speed; then mix 30mL of absolute ethanol and 5mL of TEOS to obtain solution B; In the magnetically stirred solution A, react for 24 hours after the titration is completed; repeatedly ultrasonically wash with absolute ethanol until neutral, centrifuge, and vacuum-dry at 60°C until constant weight.

Embodiment 2

[0033] Example 2. Preparation of molecularly imprinted polymer SiO on the surface of metsulfuron-methyl silica gel 2 @MSM-MIP 1

[0034] (1) Add 0.2g SiO 2 Ultrasonic disperse the pellets in 40mL toluene solution, add 2mL γ-MPTS, pass N 2 Deoxygenation, magnetic stirring at 300rpm, reaction at 100°C for 12h, repeated ultrasonic washing with methanol, centrifugation to remove unreacted γ-MPTS, vacuum drying at 60°C to constant weight;

[0035] (2) Add 0.625mmol of MSM and 2.5mmol of MAA into 25mL of acetonitrile, mix well, shake well, and let stand for 4h to prepare a pre-assembly solution;

[0036] (3) 0.1g modified SiO 2 Ultrasonically disperse the beads in 25mL acetonitrile, add 5mmol EGDMA, 0.125mmol AIBN and the pre-assembly solution prepared in step (2), ultrasonicate for 5min in an ice bath, and pass N under magnetic stirring 2 Deoxygenation, temperature controlled heating to initiate polymerization, the heating program is as follows: react at 50°C for 6 hours, heat ...

Embodiment 3

[0040] Example 3. Preparation of molecularly imprinted polymer SiO on the surface of metsulfuron-methyl silica gel 2 @MSM - MIP 2

[0041] (1) Add 0.2g SiO 2 Ultrasonic disperse the pellets in 40mL toluene solution, add 2mL γ-MPTS, pass N 2 Deoxygenation, magnetic stirring at 300 rpm, reaction at 120°C for 12 hours, repeated ultrasonic washing with methanol, centrifugation to remove unreacted γ-MPTS, vacuum drying at 60°C to constant weight;

[0042] (2) Add 0.625mmol of MSM and 2.5mmol of MAA into 25mL of acetonitrile, mix well, shake well, and let stand for 4h to prepare a pre-assembly solution;

[0043] (3) 0.1g modified SiO 2 Ultrasonically disperse the beads in 25mL acetonitrile, add 5mmol EGDMA, 0.125mmol AIBN and the pre-assembly solution prepared in step (2), ultrasonicate for 5min in an ice bath, and pass N under magnetic stirring 2 Deoxygenation, temperature controlled heating to initiate polymerization, the heating program is as follows: react at 50°C for 6 hour...

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Abstract

The invention relates to a preparation method of a molecularly imprinted polymer on nano-silica gel surfaces of sulfonylurea herbicides, which comprises the following steps: preparing SiO2 pellets; ultrasonically dispersing the prepared SiO2 pellets into a toluene solution of gamma-methacryloxypropyl trimethoxy silane, and carrying out backflow reaction to obtain modified SiO2 pellets; adding template molecules and functional monomers into a polymerization solvent and fully shaking up to obtain a pre-assembled solution; ultrasonically dispersing the modified SiO2 pellets into the polymerization solvent, and adding cross-linking agent, initiating agent and the pre-assembled solution; mixing, carrying out ice bath ultrasonic treatment, stirring, introducing N2 for removing oxygen, carrying out temperature programming thermal-initiated polymerization under the N2 atmosphere, centrifuging and removing supernatant liquid; and ultrasonically washing precipitates sequentially with a methanol-acetic acid solution and methanol to obtain polymer pellets the template molecules of which are removed. The molecularly imprinted polymer pellets prepared by the invention not only have specific recognition capability for the template molecules and analogs thereof but also have excellent characteristics of enrichment and recovery, thus the molecularly imprinted polymer pellets can be used as dispersed solid phase extraction materials for separating and enriching the sulfonylurea herbicides in environment, food and other complex samples.

Description

technical field [0001] The invention relates to a method for preparing surface-modified nano-silica gel beads, and also relates to a method for carrying out surface molecular imprinting on the nano-silica gel for sulfonylurea herbicides. Background technique [0002] The emergence of sulfonylurea herbicides is a sign that herbicides have entered the era of super high efficiency, which makes the amount of herbicides from the previous 1-3kg a.i. / hm 2 Change to 1-150g a.i. / hm 2 . This type of herbicide has a broad herbicidal spectrum, can effectively control broad-leaved weeds, has a wide application time range, and has low toxicity to mammals. Due to the advantages of such herbicides as ultra-high efficiency, low dosage, and low toxicity, such herbicides are widely used, but precisely because of the expansion of their usage and scope, their residues in crops and their toxicity to human health It is also attracting more and more attention. Therefore, the detection and contr...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
Inventor 都述虎彭艳陆庆罗晶谢颖陈雪梅陈丹君聂力陈丽娜李飞
Owner NANJING MEDICAL UNIV
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