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Graphene/silica gel solid extraction material and application thereof

A solid-phase extraction material, graphene technology, applied in material separation, analysis of materials, other chemical processes and other directions, can solve the problems of narrow pH applicable range, cumbersome detection steps, reduced detection accuracy, etc., to improve detection accuracy, Good adsorption and stability, wide applicability

Active Publication Date: 2017-10-20
淄博海关综合技术服务中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the commonly used graphene solid-phase extraction materials need to adjust the extraction solution to a certain pH range during use. The applicable range of pH is narrow, which makes the detection steps cumbersome and reduces the detection accuracy.

Method used

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  • Graphene/silica gel solid extraction material and application thereof
  • Graphene/silica gel solid extraction material and application thereof
  • Graphene/silica gel solid extraction material and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Preparation process of graphene colloidal solution

[0037] Dissolve 0.500g of graphene oxide with a particle size of less than 10 μm in 100ml of distilled water for 30 minutes, add 0.050g of PSS, stir and react at room temperature for 60 minutes, then 1.25mL of hydrazine hydrate (80%) is added to the above-mentioned graphene oxide colloidal aqueous solution, and then the whole The reaction system was placed in an oil bath at 100° C. for reflux reaction for 24 hours to prepare a graphene colloid solution.

[0038] 2) Preparation process of graphene silica gel solid phase extraction material

[0039] Add 0.250g of amino silica gel with a particle size of 2-6μm into 100ml of distilled water, ultrasonically disperse for 30min, adjust the pH of the solution to about 3 with dilute hydrochloric acid (0.1mol / L), add 25ml of graphene colloid solution (5.0mg / ml ) into the amino silica gel suspension, and the mixed solution was reacted in a water bath shaker at 50°C for 5h to...

Embodiment 2

[0041] 1) Preparation process of graphene colloidal solution

[0042] Dissolve 1.000g of graphene oxide with a particle size of less than 10 μm in 100ml of distilled water for 30 minutes, add 0.100g of PSS, stir and react at room temperature for 60 minutes, then 1.25mL of hydrazine hydrate (80%) is added to the above graphene oxide colloidal aqueous solution, and then the whole The reaction system was placed in an oil bath at 100° C. for reflux reaction for 24 hours to prepare a graphene colloid solution.

[0043] 2) Preparation process of graphene silica gel solid phase extraction material

[0044]Add 0.500g of amino silica gel with a particle size of 2-6μm to 100ml of distilled water, ultrasonically disperse for 30min, adjust the pH of the solution to 2 with dilute hydrochloric acid (0.1mol / L), add 50ml of graphene colloid solution (10.0mg / ml) Into the amino silica gel suspension, the mixed solution was reacted in a water bath shaker at 50°C for 5h to ensure that they were ...

Embodiment 3

[0046] 1) Preparation process of graphene colloidal solution

[0047] Dissolve 2.000 g of graphene oxide with a particle size of 10-20 μm in 100 ml of distilled water and ultrasonically for 30 min, add 0.200 g of PSS, stir and react at room temperature for 60 min, then 1.25 mL of hydrazine hydrate (80%) is added to the above graphene oxide colloidal aqueous solution, Then whole reaction system was placed in 100 DEG C of oil baths and reflux reaction prepared graphene colloid solution after 24 hours.

[0048] 2) Preparation process of graphene silica gel solid phase extraction material

[0049] Add 1.000g of amino silica gel with a particle size of 5-10μm to 100ml of distilled water, ultrasonically disperse for 30min, adjust the pH of the solution to 4 with dilute hydrochloric acid (0.1mol / L), add 100ml of graphene colloid solution (20mg / ml) to In the amino silica gel suspension, the mixed solution was reacted in a water bath shaker at 50°C for 5h to ensure that they were comp...

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Abstract

A graphene / silica gel solid extraction material and application thereof belong to the field of analytical detection pretreatment of composites and agricultural products. The graphene / silica gel solid extraction material prepared via an electrostatic adsorption technique is provided herein; the graphene / silica gel solid extraction material can well adsorb carbamate pesticides in plants and agricultural products by the aid of pi-pi bond action and interaction between electrostatic adsorption and carbamate pesticides; recycling experiments prove that the graphene / silica gel solid extraction material can adsorb carbamate pesticides for agricultural products under high speed and efficiency, has good detection reproducibility and high stability, has wide range of application and other advantages, and has a promising application prospect.

Description

technical field [0001] The invention discloses a graphene / silica gel solid-phase extraction material and its application, belonging to the field of composite materials and agricultural product analysis and detection pretreatment. Background technique [0002] Due to the great harm of pesticide residues to the human body, strict limit requirements have been imposed on different food and agricultural products at home and abroad. [0003] At present, the common methods for the analysis of pesticide residues are QuEChERS or solid phase extraction (SPE) pretreatment technology combined with high performance liquid chromatography or high performance liquid chromatography-tandem mass spectrometry and other detection technologies. However, experiments have found that the above pretreatment methods have low extraction rates of QuEChERS or SPE materials due to the complex composition of the actual sample matrix, so it is difficult to detect or have low sensitivity by conventional meth...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/26B01J20/30B01D15/08G01N30/02
CPCB01D15/08B01J20/265B01J20/286G01N30/02
Inventor 刘胜王利涛许健刘永强孙计赞张引
Owner 淄博海关综合技术服务中心
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