Triazole pesticide molecularly imprinted polymer microspheres, solid-phase extraction column and application of solid-phase extraction column

A technology of molecular imprinting and triazoles, which is applied in the fields of alkali metal compounds, separation methods, and other chemical processes, can solve the problem of poor hydrophilic performance and cannot extract high water content of vegetable and fruit matrices, weak class-specific recognition ability, polymer To solve problems such as poor adsorption uniformity, achieve excellent adsorption performance, high selectivity and adsorption, class specificity, and uniform particle size

Active Publication Date: 2017-01-11
BEIJING PURKINJE GENERAL INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] These methods all use the traditional bulk polymerization method, which needs to be ground and sieved. The polymers have disadvantages such as poor adsorption uniformity and weak class-specific recognition ability. Poorly unable to extract vegetable and fruit matrices with high water content, and not suitable for the enrichment and extraction of paclobutrazol and uniconazole, which are the most widely used triazole pesticides

Method used

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  • Triazole pesticide molecularly imprinted polymer microspheres, solid-phase extraction column and application of solid-phase extraction column
  • Triazole pesticide molecularly imprinted polymer microspheres, solid-phase extraction column and application of solid-phase extraction column

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Experimental program
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Effect test

Embodiment 1

[0063] A), 0.0145g triadimefon template molecule (0.05mmol) and 0.07mL methacrylic acid (0.35mmol) were dissolved in 20mL acetonitrile, and oscillated in a shaker for 25min;

[0064] B), after pre-polymerization of the template molecule and methacrylic acid, add 0.1824mL TRIM (final concentration 0.6mmol) and 30.0mg AIBN to the mixture in A) and mix thoroughly. Sealed after filling with nitrogen to remove oxygen;

[0065] C), heating in a constant temperature water bath at 55°C for 26 hours, cooling, centrifuging, sieving, discarding the supernatant to obtain a precipitate, and then drying the precipitate naturally;

[0066] D), elution with a mixed solution of acetic acid and methanol with a volume ratio of 1:9 to remove residual monomers and crosslinking agents, and then wash with methanol for 5 hours to remove acetic acid until no triadimefon is detected by high performance liquid chromatography ;

[0067] Drying the powder from which template molecules have been eluted a...

Embodiment 2

[0070] A), 0.0435g triadimefon template molecule (0.15mmol) and 0.15mL methacrylic acid (0.75mmol) were dissolved in 20mL acetonitrile, and oscillated in a shaker for 35min;

[0071] B), after pre-polymerization of template molecules and methacrylic acid, add 0.4256mL TRIM (final concentration 1.4mmol) and 30.0mg AIBN to the mixture in A) and mix thoroughly. Sealed after filling with nitrogen to remove oxygen;

[0072] C), heating in a constant temperature water bath at 65°C for 22 hours, cooling, centrifuging, sieving, discarding the supernatant to obtain a precipitate, and then drying the precipitate naturally;

[0073] D), elution with a mixed solution of acetic acid and methanol with a volume ratio of 1:9 to remove residual monomers and crosslinking agents, and then wash with methanol for 5 hours to remove acetic acid until no triadimefon is detected by high performance liquid chromatography ;

[0074] Drying the powder from which template molecules have been eluted and ...

Embodiment 3

[0077] A), 0.029g triadimefon template molecule (0.1mmol) and 0.12mL methacrylic acid (0.6mmol) were dissolved in 20mL acetonitrile, and oscillated in a shaker for 30min;

[0078] B), after pre-polymerization of the template molecule and methacrylic acid, add 0.304 mL TRIM (final concentration 1.0 mmol) and 30.0 mg AIBN to the mixture in A) and mix thoroughly. Sealed after filling with nitrogen to remove oxygen;

[0079] C), heating in a constant temperature water bath at 60°C for 24 hours, cooling, centrifuging, sieving, discarding the supernatant to obtain a precipitate, and then drying the precipitate naturally;

[0080] D), elution with a mixed solution of acetic acid and methanol with a volume ratio of 1:9 to remove residual monomers and crosslinking agents, and then wash with methanol for 5 hours to remove acetic acid until no triadimefon is detected by high performance liquid chromatography ;

[0081] Drying the powder from which template molecules have been eluted an...

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Abstract

The invention relates to the field of compound extraction and separation purification, in particular to triazole pesticide molecularly imprinted polymer microspheres, a solid-phase extraction column filled with the riazole pesticide molecularly imprinted polymer microspheres and application of solid-phase extraction column. The triazole pesticide molecularly imprinted polymer microspheres are prepared by using triadimefon as the template molecule, methacrylic acid as the functional monomer, trimethylolpropane trimethyl acrylate as the crosslinking agent and azodiisobutyronitrile as initiator to perform reaction in an inert solvent and then removing the template molecule.

Description

technical field [0001] The invention relates to the field of compound extraction and separation and purification, in particular to a triazole pesticide molecularly imprinted polymer microsphere, a solid phase extraction column and applications thereof. Background technique [0002] Triazole pesticides have shown great potential in controlling pests and diseases since their appearance in the 1970s. Triazole pesticides are mainly fungicides, which generally have the characteristics of high efficiency, low toxicity, low residue, long-lasting effect, and strong systemic absorption. In addition, triazoles are widely used as plant growth regulators at home and abroad, especially the application of paclobutrazol. [0003] The residual time of triazole pesticides in soil is generally longer, and its metabolism mainly depends on photolysis and microbial degradation. Although triazole pesticides have low toxicity and low residue, and are relatively safe for humans and animals, if th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08J9/28B01J20/26B01J20/28B01J20/30B01D15/20
CPCB01D15/20B01J20/268B01J20/28021C08F222/10C08J9/28C08J2201/0502C08J2335/02C08F222/103C08F220/06
Inventor 佘永新王静赵风年张超王珊珊金茂俊金芬邵华郑露飞
Owner BEIJING PURKINJE GENERAL INSTR
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