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Pretreatment method for pesticide residue detection in biological sample and application thereof

A technology for pesticide residue detection and biological samples, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of sample loss, limited sample processing speed, and the inability to achieve a large number of effective removal of proteins, lipids and other components, and achieve improved The effect of detection accuracy, prevention of sample loss, and shortening of pretreatment time

Active Publication Date: 2019-02-01
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

This pretreatment method still adopts the method of centrifuging the acetonitrile extract, which will still cause sample loss during the transfer process and limit the sample processing speed
In this pretreatment method, Fe 3 o 4 -SiO 2 As a magnetic adsorbent, the function is only for magnetic separation, and it cannot achieve a large amount of effective removal of proteins, lipids and other components in environmental samples
[0005] Chinese patent CN201710089362.6 discloses a sample pretreatment method for the detection of pesticide residues in fruits and vegetables. This pretreatment method can only process fruit and vegetable samples, and is not suitable for environmental biological samples with high protein content. A cloudy solution is obtained, and the effective separation of the sample matrix and the purified solution cannot be achieved

Method used

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  • Pretreatment method for pesticide residue detection in biological sample and application thereof
  • Pretreatment method for pesticide residue detection in biological sample and application thereof
  • Pretreatment method for pesticide residue detection in biological sample and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Take the bee sample to be tested and grind it evenly under the protection of liquid nitrogen to obtain the bee homogenate. Accurately weigh 0.5g of bee homogenate into a 50ml centrifuge tube, add 2ml of water, vortex for 1min; then add 5ml of acetonitrile to mix, vortex for 1min; add 30mg of Fe to the mixture 3 o 4 -TiO 2 , 10mg GCB and 2500mg dehydration material (MgSO 4 The mass ratio to NaCl is 4 / 1), vortexed for 1 min, adsorbed by an external magnet for 3 s, pipetted 1.0 ml of the supernatant, passed through a 0.22 μm filter membrane, and analyzed by UPLC-MS / MS.

Embodiment 2

[0051] Homogenize the shrimp sample to be tested to obtain the homogenate of shrimp. Accurately weigh 0.5g of shrimp homogenate in a 50ml centrifuge tube, add 2ml of water, vortex for 1min; then add 5ml of acetonitrile to mix, vortex for 1min; add 30mg of Fe to the mixture 3 o 4 -TiO 2 , 10mgGCB and 2500mg water removal material (MgSO 4 The mass ratio to NaCl is 4 / 1), vortexed for 1 min, adsorbed by an external magnet for 3 min, pipetted 1.0 ml of the supernatant, passed through a 0.22 μm filter membrane, and analyzed by UPLC-MS / MS.

Embodiment 3

[0053] Homogenize the fish sample to be tested to obtain fish homogenate. Accurately weigh 0.5g of fish homogenate into a 50ml centrifuge tube, add 2ml of water, vortex for 1min; then add 5ml of acetonitrile to mix, vortex for 1min; add 30mg of Fe to the mixture 3 o 4 -TiO 2 , 10mgGCB and 25mg dehydration material (MgSO 4 The mass ratio to NaCl is 4 / 1), vortexed for 1 min, adsorbed by an external magnet for 3 s, pipetted 1.0 ml of the supernatant, passed through a 0.22 μm filter membrane, and analyzed by UPLC-MS / MS.

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Abstract

The invention provides a pretreatment method for pesticide residue detection in a biological sample, and relates to the field of pesticide residue analysis in environmental organism. The method comprises the following steps: mixing a homogenate of a biological sample to be detected with water to obtain a first mixture; mixing the first mixture directly with acetonitrile for adsorption, and obtaining a second mixture comprising an acetonitrile layer and a water layer; mixing the second mixture directly with a purified adsorption material, and reacting for more than 1 min; and aggregating the purified adsorption material by external magnetic field adsorption, separating a supernatant for filtration, and the obtained filtrate is a to-be-detected liquid for pesticide residue detection. The purified adsorption material comprises Fe3O4-TiO2, GCB, MgSO4 and NaCl. According to the pretreatment method for the pesticide residue detection in the biological sample, a suitable water addition ratiofor the biological sample having high protein content and complex impurity components is provided. In the process of the pretreatment method of the invention, the purification and extraction steps arecombined to shorten the time and improve the detection precision, and high-throughput detection can be realized.

Description

technical field [0001] The invention relates to the technical field of analyzing pesticide residues in environmental organisms, in particular to a pretreatment method for detecting pesticide residues in biological samples and an application thereof. Background technique [0002] With the increasing application of pesticides, the problem of pesticide residues in environmental organisms has attracted more and more attention. Environmental organisms contain complex components and high protein content. In order to obtain reliable detection results, it is necessary to eliminate the interference of other components in environmental organisms on the detection results. In recent years, the sample extraction methods commonly used in the analysis of pesticide residues in environmental organisms include: solvent extraction (SE), supercritical fluid extraction (SFE), and purification methods include: solid phase extraction (SPE), matrix solid phase dispersion Generally, samples need to...

Claims

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Application Information

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IPC IPC(8): G01N30/06
CPCG01N30/06
Inventor 齐沛沛王新全王祥云汪志威苍涛王强
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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