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Preparation method and application of functional magnetic graphene ionic liquid adsorbent

A functional bromide ion technology, applied in the field of chemical analysis and detection, can solve the problems of simultaneous qualitative and quantitative analysis of preservatives, excessive use of organic solvents, complex matrix, etc., and achieve shortened detection time, short extraction time, and organic solvents. The effect of using less

Inactive Publication Date: 2018-05-04
INSPECTION & QUARANTINE TECH CENT OF CHONGQING ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0005] When the traditional solid phase extraction (SPE) adsorbent is used for pretreatment of the sample, it needs to be packed into a column and loaded with a large volume of sample, which causes problems such as time-consuming, easy to clog, large amount of organic solvent and cumbersome operation;
[0006] The vegetable sample matrix is ​​complex, and the adsorbent often adsorbs more impurities while adsorbing the target substance. The adsorbent used in the existing pretreatment technology cannot achieve specific adsorption on the preservative with a specific structure. Simultaneous qualitative and quantitative analysis of multiple components is limited

Method used

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  • Preparation method and application of functional magnetic graphene ionic liquid adsorbent
  • Preparation method and application of functional magnetic graphene ionic liquid adsorbent
  • Preparation method and application of functional magnetic graphene ionic liquid adsorbent

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preparation example Construction

[0058] The preparation method of the functional IL provided by the embodiment of the present invention comprises the following steps:

[0059] (1) 1.0g 2-sodium naphthalenesulfonate and 1.0g 1-vinyl-3 octyl-imidazole bromide (VOIm + Br - ) were dissolved in 200 mL of water respectively, and then the two solutions were mixed and mechanically stirred overnight.

[0060] (2) 250mL of chloroform was added to the separatory funnel equipped with the mixed solution to extract IL (1-vinyl-3 octyl-imidazole-2-naphthalenesulfonate), repeat the operation once, and combine the lower layer extraction twice solution.

[0061] (3) Add 300 mL of double distilled water to the separatory funnel containing the extraction solution to wash the extraction solution several times to remove bromide ions until no bromide ions are detected in the aqueous phase.

[0062] (4) The chloroform was removed from the IL extraction solution by a rotary evaporator to obtain the functional IL, which was dried u...

Embodiment 1

[0094] (1) Preparation of magnetic Fe 3 o 4 Nanoparticles:

[0095] Accurately weigh 3.40g of ammonium ferrous sulfate hexahydrate and 8.35g of ferric sulfate dodecahydrate into 400mL of water at 50°C, then add 20mL of ammonia water dropwise to precipitate iron oxide, and sonicate for 10min to adjust the pH to 11. The mixed solution was stirred for 2 h to obtain a precipitate. The precipitate was washed with first-grade water to pH 7, the obtained precipitate was dispersed in water, 1.7 mL of polyvinylpyrrolidone (PVP) was added to the mixture, and stirred at room temperature for 1 day to obtain Fe 3 o 4 nanospheres.

[0096] (2) Preparation of Fe 3 o 4 @SiO 2 :

[0097] 1.4g Fe 3 o 4 Pour the microspheres into a mixed solution containing 280mL ethanol and 70mL water, and add 5mL ammonia water. After stirring for 15 min, 4 mL of tetraethylorthosilicate (TEOS) was added dropwise. Stirring at room temperature for 8 h, the product was separated by an external magnetic...

Embodiment 2

[0109] Each process is all carried out according to embodiment 1, only the consumption of IL in the step (7) is changed into 0.2g.

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Abstract

The invention belongs to the field of chemical analysis and detection and discloses a preparation method and an application of a functional magnetic graphene ionic liquid adsorbent. A novel magnetic adsorbent is synthesized by synthesizing a line of an ionic liquid. Compared with conventional solid phase extraction (SPE) column filler, a Fe3O4@SiO2@G@IL adsorbent has functional groups and a largespecific surface area, can be quickly separated and can adsorb targets specifically, so that the adsorbent has a relatively good extraction ability and extraction efficiency. The prepared Fe3O4@SiO2@G@IL is taken as an adsorbent of magnetic solid extraction (MSPE), and eight preservatives: myclobutanil, propiconazole, triadimefon, methiocarb, benalaxyl, fenamiphos, fenbuconazole and triadimenol can be measured at the same time. The result shows that the Fe3O4@SiO2@G@IL prepared by the invention has a specific adsorption effect on the eight preservatives which have good recovery rates and precision.

Description

technical field [0001] The invention belongs to the field of chemical analysis and detection, in particular to a preparation method and application of a functional magnetic graphene ionic liquid adsorbent. Specifically related to a functional Fe 3 o 4 @SiO 2 Preparation of @G@IL adsorbent and its application in the determination of eight preservative residues in vegetables by ultra-high liquid chromatography-tandem mass spectrometry. Background technique [0002] Vegetables are rich in vitamins, minerals and dietary fiber, which can supplement the nutrients needed by the human body. Due to the short fresh-keeping time of vegetables, it is not conducive to transportation and storage. Preservatives are usually added to prevent vegetables from rotting. However, most of the chemical preservatives are pesticides. In the process of vegetable preservation, the phenomenon of abuse, misuse, and excessive residue has seriously threatened the health of consumers and caused some ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/28B01J20/30B01D15/38G01N30/02G01N30/06
CPCB01D15/3885B01J20/28009B01J20/281G01N30/02G01N30/06G01N2030/062
Inventor 曹淑瑞郗存显陈久燕唐柏彬张雷李贤良王国民
Owner INSPECTION & QUARANTINE TECH CENT OF CHONGQING ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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