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Method for determining imidacloprid, sulfluramid and metabolites thereof

A technology of imidacloprid and sulfluramid, which is applied in the field of analytical chemistry, can solve the problems of time-consuming and laborious, large pre-treatment sampling amount, and many extraction solvents, etc., and achieves the effects of simple pre-treatment, small sampling amount, and low usage amount.

Pending Publication Date: 2022-07-29
CAS CENT FOR EXCELLENCE IN MOLECULAR PLANT SCI
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] In the existing detection methods of imidacloprid and sulfluramid residues in soil, the pretreatment sampling volume is large, generally 10g of soil needs to be taken, and the extraction solvents used are many, generally more than 20mL are needed to extract imidacloprid, sulfluramid and sulfluramid in the soil. Its metabolites are time-consuming and labor-intensive

Method used

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  • Method for determining imidacloprid, sulfluramid and metabolites thereof
  • Method for determining imidacloprid, sulfluramid and metabolites thereof
  • Method for determining imidacloprid, sulfluramid and metabolites thereof

Examples

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Embodiment 1

[0052] Example 1: Determination of imidacloprid and sulfluramid and their metabolites in soil

[0053] 1. Sample pretreatment

[0054] Preparation of extraction solvent: acetonitrile: water ≈ 1:1 (v / v), plus 5% formic acid;

[0055] Soil extraction: Weigh 0.2 g of freeze-dried soil, add 400 μL of extraction solvent, vortex for 1 min, shake for 10 min, centrifuge for 10 min, and take 100 μL of supernatant to obtain soil extraction samples. Add 100 μL of pure water, mix well and centrifuge for 10 min, take the supernatant to obtain a liquid sample for loading, and perform LC-MS / MS detection.

[0056] 2. LC-MS / MS detection

[0057] Instrument: ExionLC TM AD+QTRAP 6500 plus

[0058] liquid phase method

[0059] Chromatographic column: Agilent XBD C18 (100mm*3mm, 1.8μm);

[0060] Column temperature: 40℃;

[0061] Injection volume: 1 μL;

[0062] Aqueous phase A: an aqueous solution containing 2 mM ammonium formate and 0.01% formic acid;

[0063] Organic phase B: methanol ...

Embodiment 2

[0085] Example 2: Detection of matrix effects

[0086] Using soil without pesticide residues as raw material, prepare matrix solvent as follows: Weigh 0.2 g of lyophilized soil, add 400 μL of extraction solvent (acetonitrile: water = 1:1 v / v, containing about 5% formic acid), vortex Spin for 1 min, shake for 10 min, centrifuge for 10 min, take the supernatant, add the same amount of pure water, mix well, centrifuge for 10 min, take the supernatant to obtain the matrix solvent.

[0087] The blank solvent was prepared according to the following method: acetonitrile:water=1:3 (v / v) solution was the blank solvent.

[0088] The above solvents were used to prepare the concentrations of each compound to be 0.01ng / mL, 0.05ng / mL, 0.1ng / mL, 0.5ng / mL, 1ng / mL, 5ng / mL, 10ng / mL, 50ng / mL, 100ng / mL, 500ng / mL and 1000ng / mL matrix standard and solvent standard, enter LC-MS / MS detection, record the peak area, fit the matrix standard curve and solvent standard curve, divide the slope of the matr...

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Abstract

The invention discloses a method for determining imidacloprid, sulfluramid and metabolites thereof, which comprises the following steps: (1) detecting a liquid sample comprising at least one of imidacloprid, sulfluramid and metabolites thereof by adopting a liquid chromatography tandem triple quadrupole, wherein the mobile phases adopted in the liquid chromatography are respectively an aqueous phase A, namely an aqueous solution containing 0.5-4mM of ammonium formate and 0.005-0.02% of formic acid; an organic phase B: a methanol solution containing 0.5-4 mM of ammonium formate and 0.005-0.02% of formic acid; and (2) determining the content of each compound according to the standard curve of each compound. The method has the advantages of small sampling amount, simple pretreatment and small use amount of organic reagents, and can be used for simultaneously detecting two pesticides, namely imidacloprid and sulfluramid, and 10 compounds, namely metabolites of imidacloprid and sulfluramid.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a method for determining imidacloprid, sulfluramid and their metabolites, in particular to a method for determining imidacloprid, sulfluramid and their metabolites in soil by using LC-MS / MS. Background technique [0002] Pesticide residues refer to the amount of pesticides and their toxic metabolites that remain in plants, soil and the environment after the use of pesticides. Imidacloprid and sulfluramid are commonly used nitromethylene pesticides, which are toxic and easily remain in plants and accumulate through the food chain, thereby causing environmental pollution and endangering human health. In order to ensure environmental safety and food safety, the establishment of a rapid and reliable method for the detection of imidacloprid and sulfluramid is of great significance to protect people's health. [0003] In the existing detection methods for imidacloprid and sulfluramid ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72
Inventor 王姗姗徐晓燕胡文利
Owner CAS CENT FOR EXCELLENCE IN MOLECULAR PLANT SCI
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