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Method for detecting triazine herbicides and metabolites thereof in shellfish

A technology for metabolites and detection methods, applied in the field of pesticide residue detection in aquatic products, can solve the problems of complex operation, low accuracy, and inability to eliminate effects, and achieve the effect of simple operation and easy reproducibility.

Active Publication Date: 2020-06-09
YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The recovery rate of the external standard method is difficult to guarantee, and the accuracy is not high. The external standard method for matrix calibration cannot eliminate the influence of the pretreatment process. At the same time, it needs to be calibrated separately for different matrices, and the operation is complicated.

Method used

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  • Method for detecting triazine herbicides and metabolites thereof in shellfish
  • Method for detecting triazine herbicides and metabolites thereof in shellfish
  • Method for detecting triazine herbicides and metabolites thereof in shellfish

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Preparation of working solution

[0036] Weigh appropriate amount of triazine herbicides, metabolites and internal standard, dilute to volume with methanol, prepare 1.0 mg / mL standard stock solution respectively, and store at -18°C in the dark. Then accurately draw a certain amount of standard stock solution, dilute with methanol to prepare 1 μg / mL mixed standard external standard working solution and internal standard working solution, and store in refrigerated storage at 4°C.

[0037] (2) Efficient pretreatment

[0038] The shellfish samples were shelled and the edible part was homogenized. Weigh 2.0g of sample, add 50μL internal standard (1ppm), then add 400μL 1.5mol / L NaOH solution and mix well, use 5mL acetonitrile to extract, vortex and mix well, then sonicate for 2min, centrifuge at 4500r / min for 5min, and extract the supernatant , add 5 mL of acetonitrile to the remaining residue and repeat the extraction once, combine the two supernatants, add about 5.0 g...

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Abstract

The invention discloses a method for detecting triazine herbicides and metabolites thereof in a shellfish, and belongs to the technical field of detection of pesticide residues in aquatic products. The method for detecting triazine herbicides and metabolites thereof in the shellfish comprises the following steps: carrying out efficient pretreatment on a shellfish sample to be detected; and introducing an internal standard method and combining high-performance liquid chromatography-quadrupole tandem mass spectrometry and high-resolution mass spectrometry to quantitatively and qualitatively analyze the triazine herbicides and metabolites thereof in the shellfish sample. The sample pretreatment method provided by the invention can quickly remove a large amount of fat interference in the sample, and the method is simple to operate, and the reproduction is easy. The internal standard method is combined with the high-performance liquid chromatography-quadrupole tandem mass spectrometry and high-resolution mass spectrometry, and the triazine herbicides and metabolites thereof in shellfish samples are rapidly, quantitatively, accurately and qualitatively analyzed.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection in aquatic products, and specifically relates to an internal standard method combined with high-performance liquid chromatography-quadrupole tandem mass spectrometry and high-resolution mass spectrometry for qualitative and quantitative detection of triazine herbicides in shellfish and their metabolism product method. Background technique [0002] Triazine herbicides are selective herbicides widely used in agricultural production and aquaculture to control the growth of weeds and algae. Because of its high herbicidal effect, it has been widely and overused worldwide, and its chemical properties are stable and difficult to degrade, resulting in its rapid accumulation in soil and water. Entering the environmental system through surface runoff and discharge has become the main source of ecological environmental pollution. Due to the long half-life and high toxicity of triazine h...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/36G01N30/86
CPCG01N30/02G01N30/06G01N30/36G01N30/8679G01N2030/062
Inventor 孙晓杰李兆新高金芳谭杰刘佳敏郭萌萌谭志军王联珠翟毓秀
Owner YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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