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A method for the determination of three phenoxycarboxylic acid pesticide residues in tobacco by ultra-high performance convergence chromatography-tandem mass spectrometry

An ultra-efficient convergence and pesticide residue technology, which is applied in the field of ultra-efficient convergence chromatography-tandem mass spectrometry for the determination of three phenoxycarboxylic acid pesticide residues in tobacco, and achieves improved sensitivity and repeatability, accurate quantification, and high accuracy. Simple processing effect

Active Publication Date: 2020-01-17
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Application Information

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Problems solved by technology

No reports have been found on the use of ultra-performance convergence chromatography-tandem mass spectrometry (UPC 2 -MS / MS) Determination of Phenoxyacetic Acid Herbicides in Tobacco

Method used

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  • A method for the determination of three phenoxycarboxylic acid pesticide residues in tobacco by ultra-high performance convergence chromatography-tandem mass spectrometry
  • A method for the determination of three phenoxycarboxylic acid pesticide residues in tobacco by ultra-high performance convergence chromatography-tandem mass spectrometry
  • A method for the determination of three phenoxycarboxylic acid pesticide residues in tobacco by ultra-high performance convergence chromatography-tandem mass spectrometry

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Experimental program
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Effect test

example 1

[0029] 1. Instruments and reagents:

[0030]Pesticides: 2,4-D, 2,4,5-T and dicamba, and their corresponding deuterated internal standards are standard products (purity greater than 98%); methanol and dichloromethane are pesticide residue grade, hydrochloric acid For analytical purity.

[0031] Waters Convergence Chromatography-Tandem Quadrupole Mass Spectrometer; Vortex Oscillator (Labnet, USA); AE 163 Electronic Balance (Sensitivity: 0.0001g) (Mettler, Switzerland).

[0032] 2. Sample handling:

[0033] Weigh 1.0 g sample, place it in a 50 mL stoppered centrifuge tube, add 10 mL 0.5moL / L hydrochloric acid aqueous solution and 10 mL CH 2 Cl 2 , and add 100 μL mixed internal standard working solution, and vortex for 15 minutes. Pipette 1 mL of the lower organic phase, blown to dryness with nitrogen, redissolve in methanol, and put into UPC 2 - MS / MS detection;

[0034] 3. Prepare the standard working solution: Weigh 0.01 g of 2,4-D, 2,4,5-T and dicamba three pesticide s...

example 2

[0038] Example 2: According to the method described in Example 1, another tobacco leaf sample was selected, and the detection amount of dicamba in the sample was 0.12 mg / kg.

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Abstract

The invention provides a method for determining the residual amount of three phenoxycarboxylic acid pesticides in tobaccos by adopting an ultrahigh performance convergence chromatography-tandem mass spectrometry. The method is characterized by comprising the following steps: extracting a sample by utilizing a 0.5mol / L hydrochloric acid solution; carrying out back extraction by adopting dichloromethane and determining the residual amount of the pesticides including 2,4-D, 2,4,5-T and dicamba in the tobaccos by adopting the ultrahigh performance convergence chromatography-tandem mass spectrometry. By adopting the method provided by the invention, the disadvantages of a sample treatment method in the prior art are overcome; a sample pre-treatment method and instrument detection conditions aiming at tobacco samples are optimized; compared with the prior art, the method provided by the invention has the following good effects that a sample pre-treatment process of the method is simple and rapid and derivatization is not needed; the method is green and environmentally friendly and has the advantages of accuracy in operation, high sensitivity and good repeatability.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical inspection of pesticide residues in tobacco and tobacco products, and mainly relates to three chlorophenoxycarboxylic acid pesticide residues in tobacco and tobacco products, including 2,4-D, 2,4,5-T and dicamba. Quantitative method. Background technique [0002] The safety of phenoxycarboxylic acid herbicides on crops is greatly affected by environmental conditions and crop growth period, and improper application may cause serious phytotoxicity. In the process of use, it is found that it has a certain endocrine disrupting effect on humans and animals. With the increasing amount and scope of use of this type of herbicide, its residues in crops and the harm to human health and the environment are also increasing. increasingly attracting people's attention. my country and other countries have established strict residue limits. For example, Japan stipulates that 2,4,5-T cannot be dete...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 杨飞唐纲岭刘珊珊边照阳邓惠敏李中皓范子彦王颖
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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