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Solid-phase adsorption material and application thereof to QuEChERS method

A solid-phase adsorption and carbon material technology, applied in the field of analytical chemistry, can solve the problems of prolonging the analysis time and rapid detection of unfavorable samples, and achieve the effect of shortening the analysis time and facilitating rapid detection

Inactive Publication Date: 2013-01-16
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the actual operation process, this kind of adsorption material can only be separated from the extract by centrifugation or filtration, which prolongs the analysis time and is not conducive to the rapid detection of a large number of samples

Method used

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  • Solid-phase adsorption material and application thereof to QuEChERS method
  • Solid-phase adsorption material and application thereof to QuEChERS method
  • Solid-phase adsorption material and application thereof to QuEChERS method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation of embodiment 1 solid-phase adsorption material

[0031] In this example, graphitized carbon black, ethylenediamine-N-propyl bonded silane and magnetic ferric oxide particles were used to prepare solid-phase adsorption materials.

[0032] Preparation steps:

[0033] 1. Preparation of graphitized carbon black / ethylenediamine-N-propyl bonded silane / magnetic ferric oxide particle solid-phase adsorption material: graphitized carbon black, ethylenediamine-N-propyl bonded silane and The magnetic iron ferric oxide particles were washed several times with water and acetonitrile, and dried for use; weighed 100 mg graphitized carbon black, 500 mg ethylenediamine-N-propyl bonded silane and 400 mg magnetic ferric oxide particles To a 15 mL amp bottle, add 10 mL of acetonitrile; oscillate with a micro-vortex mixer for 2 min, and pour off the upper liquid with the help of an external magnetic field; the product is vacuum-dried at 40 °C for 12 h before use.

...

Embodiment 2

[0035] Example 2 Detection of Pesticide Residues in Cucumber

[0036] In this example, the improved QuEChERS method was used to detect pesticide residues in cucumber.

[0037] Detection steps:

[0038]Determination of pesticide residues in cucumber: cut the cucumber sample to be tested into small pieces, and beat it into a homogenate with a mixer; take 10 g of the homogenate into a 50 mL plastic centrifuge tube, add triphenyl phosphate internal standard to 0.1 mg / kg, and let stand for a while time. Add 10 mL of acetonitrile to the treated sample homogenate, and shake for 1 min with a micro-vortex mixer. Then add 4 g of anhydrous magnesium sulfate and 1 g of sodium chloride, vibrate with a micro-vortex mixer for 1 min, centrifuge at a speed of 5000 rpm for 5 min, and transfer the obtained supernatant to a 15 mL centrifuge tube for further water removal. Pipette 0.5 mL of the dewatered acetonitrile extract, add it into a 2 mL centrifuge tube filled with 65 mg of solid-phase ...

Embodiment 3

[0039] Example 3 Detection of Pesticide Residues in Edible Cucurbit Melon

[0040] In this example, the improved QuEChERS method was used to detect pesticide residues in edible cucurbits.

[0041] Detection steps:

[0042] Determination of pesticide residues in edible cucurbit melon: cut the edible cucurbit melon sample to be tested into small pieces, and beat it into a homogenate with a blender; take 10 g of the homogenate into a 50 mL plastic centrifuge tube, add triphenyl phosphate internal standard to 0.1 mg / kg, let stand for a period of time. Add 10 mL of acetonitrile to the treated sample homogenate, and shake for 1 min with a micro-vortex mixer. Then add 4 g of anhydrous magnesium sulfate and 1 g of sodium chloride, vibrate with a micro-vortex mixer for 1 min, centrifuge at a speed of 5000 rpm for 5 min, and transfer the obtained supernatant to a 15 mL centrifuge tube for further water removal. Pipette 0.5 mL of the dewatered acetonitrile extract, add it into a 2 m...

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Abstract

The invention discloses a solid-phase adsorption material and an application thereof to a QuEChERS method. The solid-phase adsorption material disclosed by the invention adopts a carbon material, a modified silica gel material and a magnetic ferroferric oxide composite material as adsorption materials; and the price is low and the commercialization is easy to realize. The QuEChERS method comprises the following steps of: firstly extracting sample homogenate added with salt by using acetonitrile; then adding anhydrous magnesium sulfate to remove water and using the magnetic adsorption material to remove a large amount of interference objects in the acetonitrile; and finally, directly carrying out detection and analysis on a treated solution. The magnetic adsorption material has a magnetic separation performance and can be rapidly separated from the solution under the effect of an external magnetic field; and the operation is simple and the analyzing time is effectively reduced.

Description

[0001] technical field [0002] The invention relates to a solid-phase adsorption material and its application in the QuEChERS method, belonging to the field of analytical chemistry. Background technique [0003] Pesticides play a very important role in protecting humans and livestock from infectious diseases and ensuring high crop yields. But at the same time, the unavoidable pesticide residues have caused potential threats to the health of humans and livestock and have negative impacts on the ecological environment. Therefore, a variety of analytical chemistry methods have been developed to detect pesticide residues, and their applications include environmental monitoring, regulatory enforcement, organic food certification, and foreign trade. [0004] The word QuEChERS comes from the abbreviation of Quick, Easy, Cheap, Effective, Rugged and Safe, which is a sample pretreatment method that is "quick, easy, cheap, effective, stable and safe". QuEChERS technology is mostly ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/281G01N30/06
Inventor 冯钰锜郑浩博赵琴罗彦波
Owner WUHAN UNIV
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