Pretreatment method for strong-polarity pesticide residue detection

A technology for pesticide residue detection and strong polarity, which is used in the preparation of test samples to ensure recovery, remove impurities and reduce pollution.

Inactive Publication Date: 2014-06-04
刘靖靖
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Another object of the present invention is to provide a sample pretreatment method to make up for the deficiency that the existing QuEChERS method that is widely recognized internationally cannot be used for the detection of strong polar pesticides so far

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  • Pretreatment method for strong-polarity pesticide residue detection
  • Pretreatment method for strong-polarity pesticide residue detection
  • Pretreatment method for strong-polarity pesticide residue detection

Examples

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Embodiment 1

[0030] Example 1: Detection of paraquat residues in apples

[0031] (1) Sample pretreatment

[0032] Weigh 10.0 g of the homogenized apple sample into a 50 mL stoppered plastic centrifuge tube, add 10 mL of methanol aqueous solution, vortex for 1 min, centrifuge at 5000 r / min for 5 min, and the supernatant extract is to be purified. Take 2mL of the supernatant extract into a centrifuge tube containing 100mg C18 and 100mg PSA, vortex for 1min, centrifuge at 5000r / min for 3min, and pass the supernatant through a 0.22μm filter membrane for liquid chromatography-quadrupole time-of-flight series Mass Spectrometry (LC-Q TOF) Determination.

[0033] (2) Preparation of standard working solution

[0034] Weigh 25±0.1mg of the standard product into a 25mL plastic volumetric flask, dissolve it with acetonitrile, and dilute to obtain a 1000.0μg / mL standard stock solution; pipette 1.0mL of the standard stock solution into a 100mL plastic volumetric flask, and dilute to volume with aceton...

Embodiment 2

[0050] Example 2: Detection of glufosinate-ammonium, glyphosate and aminomethyl phosphate residues in carrots

[0051] (1) Sample pretreatment

[0052] Weigh 10.0 g of the thoroughly mixed carrot sample into a 50 mL stoppered plastic centrifuge tube, add 10 mL of aqueous methanol, vortex for 1 min, and centrifuge at 5000 r / min for 5 min. After centrifugation, take 2 mL of the supernatant extract into a centrifuge tube containing 100 mg of C18, vortex for 1 min, and centrifuge at 5000 r / min for 3 min. After the supernatant was passed through a 0.22 μm filter membrane, it was derivatized.

[0053] (2) Preparation of standard working solution

[0054] Weigh 25±0.1mg of standard substance into a 25mL plastic volumetric flask, dissolve with acetonitrile, and dilute to get 1000.0μg / mL standard stock solution; pipette 1.0mL each of glufosinate-ammonium, glyphosate and aminomethylphosphoric acid standard stock solution Place in a 100mL plastic volumetric flask, and dilute to volume...

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Abstract

The invention discloses a pretreatment method for strong-polarity pesticide residue detection. The pretreatment method comprises the steps of extracting strong-polarity pesticides from a sample through a methanol aqueous solution, purifying an extracting solution through a dispersive solid-phase extraction agent, and filtering the extracting solution for instrument analysis. The pretreatment method disclosed by the invention is a complementation and an improvement on the existing QuEChERS method, so that the shortcoming that the conventional internationally accepted QuEChERS method cannot be used for detecting the strong-polarity pesticides is overcome. The pretreatment method is easy to operate and high in reproducibility; the recycling rate of a strong-polarity compound is effectively guaranteed; meanwhile, impurities in the sample extracting solution are effectively removed during purification, so that pollution to a detection instrument is relieved, and the detection sensitivity is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of determination of pesticide residues, in particular to a pretreatment method for determination of highly polar pesticide residues. Background technique [0002] The QuEChERS method is a sample pretreatment method that represents fast, simple, cheap, efficient, stable and safe (Quick, Easy, Cheap, Effective, Rugged, Safe). In 2003, scientists from the United States Department of Agriculture (USDA) proposed the QuEChERS method for pesticide analysis for the first time. Laboratories such as the US FDA and the European Union have also participated in research and formulated standard methods, which have been continuously revised and improved. At present, QuEChERS methods that are widely used in the world include EN15662 developed by the European Union and AOAC2007.01 standard method of the American Association of Official Analytical Chemists. The above methods all include two steps of extraction and purificati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/34
Inventor 刘靖靖汤志旭王骏
Owner 刘靖靖
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