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Magnetic fullerene nano-material and application thereof in magnetic dispersion solid-phase extraction of methyl methoxyacrylate pesticides

A technology of methyl methoxyacrylate and magnetic fullerene, which can be used in material separation, analysis of materials, other chemical processes, etc., can solve the problems of complicated operation steps, difficult recycling of adsorbents, long time consumption, etc., and achieves good selectivity. , save processing time and cost, method fast effect

Active Publication Date: 2020-09-29
合肥海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the shortcomings of traditional solid-phase pretreatment methods such as cumbersome operation steps, long time consumption, and difficult recycling of adsorbents, the present invention provides a magnetic fullerene nanomaterial and its magnetically dispersed solid phase of methyl methoxyacrylate pesticides. Application in extraction, in order to achieve highly selective adsorption, separation, and detection of methyl methoxyacrylate pesticides such as azoxystrobin, pyraclostrobin, trifloxystrobin, and pyraclostrobin in the tested samples

Method used

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  • Magnetic fullerene nano-material and application thereof in magnetic dispersion solid-phase extraction of methyl methoxyacrylate pesticides
  • Magnetic fullerene nano-material and application thereof in magnetic dispersion solid-phase extraction of methyl methoxyacrylate pesticides
  • Magnetic fullerene nano-material and application thereof in magnetic dispersion solid-phase extraction of methyl methoxyacrylate pesticides

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Experimental program
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Effect test

Embodiment 1

[0033] This embodiment prepares Fe according to the following steps 3 o 4 @SiO 2 @C 60 Nanoparticles:

[0034] Step 1, 1g Fe 3 o 4 Nanoparticles were dispersed in 100mL isopropanol and 8mL water, ultrasonically dispersed for 15min, blown with nitrogen and stirred at room temperature; then added 10mL ammonia water with a mass concentration of 26%, stirred for 5min, added 8mL tetraethyl orthosilicate, and heated to 45°C Stir for 12 h; magnetically separate the product, wash with deionized water and ethanol in turn, and dry under vacuum at 60 °C for 12 h to obtain Fe 3 o 4 @SiO 2 Nanoparticles;

[0035] Step 2, the Fe synthesized in step 1 3 o 4 @SiO 2 Nanoparticles were dissolved in 100mL toluene, stirred at room temperature for 30min with nitrogen gas; then 1mL triethylamine and 2mL 3-chloropropyltrimethoxysilane were added, and the temperature was raised to 110°C to continue the reaction for 24h; cooled to room temperature, the product was magnetically separated, an...

Embodiment 2

[0040] This embodiment prepares Fe according to the following steps 3 o 4 @SiO 2 @C 60 Nanoparticles:

[0041] Step 1, 2g Fe 3 o 4 Nanoparticles were dispersed in 200mL of isopropanol and 16mL of water, ultrasonically dispersed for 15min, blown with nitrogen and stirred at room temperature; then added 20mL of ammonia water with a mass concentration of 26%, stirred for 5min, added 16mL of tetraethyl orthosilicate, and heated to 45°C Stir for 12 h; magnetically separate the product, wash with deionized water and ethanol in turn, and dry under vacuum at 60 °C for 12 h to obtain Fe 3 o 4 @SiO 2 Nanoparticles;

[0042] Step 2, the Fe synthesized in step 1 3 o 4 @SiO 2 Nanoparticles were dissolved in 200mL of toluene, stirred at room temperature for 30min with nitrogen gas; then 2mL of triethylamine and 4mL of 3-chloropropyltrimethoxysilane were added, and the temperature was raised to 110°C to continue the reaction for 24h; cooled to room temperature, the product was mag...

Embodiment 3、 application example

[0047] The above-mentioned embodiment gained Fe 3 o 4 @SiO 2 @Cl nanoparticles can be used as magnetic dispersive solid phase extraction adsorbent for magnetic dispersive solid phase extraction of methyl methoxyacrylate pesticides in water samples or fruit and vegetable samples, and combined with UHPLC-MS / MS analysis to determine the Measuring the concentration of methyl methoxyacrylate pesticides in water samples or fruit and vegetable samples. Specific steps are as follows:

[0048] Step 1. Extraction

[0049] The extraction method of the environmental water sample is as follows: draw 1mL of the water sample to be tested into a 15mL conical centrifuge tube, add 9mL of ultrapure water and mix well, then add 30mg of the magnetic fullerene nanomaterial obtained in the above examples, shake and extract for 20min; The magnetic fullerene nanomaterials gather to the bottom, pour all the solution;

[0050] The extraction method of fruit and vegetable samples is as follows: Weig...

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Abstract

The invention discloses a magnetic fullerene nano-material and application thereof in magnetic dispersion solid-phase extraction of methyl methoxyacrylate pesticides. The preparation method comprisesthe following steps: firstly, modifying Fe3O4 nanoparticles by using tetraethoxysilane (TEOS) to obtain ferroferric oxide superparamagnetic particles wrapped by silicon dioxide, wherein the silicon dioxide-coated ferroferric oxide superparamagnetic particles are marked as Fe3O4@SiO2 nanoparticles; then, enabling the Fe3O4@SiO2 nanoparticles to react with 3-chloropropyltrimethoxysilane so as to obtain Fe3O4@SiO2@Cl nanoparticles; finally, enabling fullerene C60 to react with benzaldehyde and benzylamine to obtain 2,5-diphenylfullerenepyrroline, and then enabling the 2,5-diphenylfullerenepyrroline to react with the Fe3O4@SiO2@Cl nanoparticles to obtain the magnetic fullerene nano-material which is recorded as Fe3O4@SiO2@C60 nanoparticles. The magnetic fullerene nano-material disclosed by theinvention can be used for magnetic dispersion solid-phase extraction of methyl methoxyacrylate pesticides, and is strong in adsorbability, large in adsorption capacity, good in selectivity and easy to elute.

Description

Technical field [0001] The invention belongs to the technical field of enrichment, purification and detection of pesticide residues in food and environmental samples, and specifically relates to a magnetic fullerene nanomaterial and its application in magnetic dispersion solid phase extraction of methyl methoxyacrylate pesticides. Background technique [0002] Pesticide residue analysis is a technique for analyzing trace components in complex mixtures. Less sample consumption, less reagent consumption, and fast analysis speed are the development trends of pesticide chemical pollutant residue detection technology. How to realize multi-residue analysis and effectively remove impurities while ensuring recovery rate is the difficulty of the entire pretreatment process. [0003] Magnetic solid-phase extraction technology is a new type of sample pretreatment technology developed in recent years. It has some special advantages compared with traditional solid-phase extraction: magn...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/28B01J20/30G01N30/06
CPCB01J20/281B01J20/28009B01J20/28004G01N30/06G01N2030/062
Inventor 宋伟周典兵韩芳王钰吕亚宁丁磊刘宇欣郑平郭春丽
Owner 合肥海关技术中心
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