Method for determining residual amount of three types of phenoxyalkanoic acid pesticides in tobaccos through extraction-purification synchronization method

A technology of pesticide residues and phenoxycarboxylic acids, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of different, signal response value variation, affecting detection limit, quantitative limit accuracy and precision, etc. Achieve quantitative accuracy, reduce the use of organic solvents, and shorten the pre-extraction treatment time

Inactive Publication Date: 2018-06-19
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the existence of some interfering components in the matrix, the ion generation speed of the component to be measured is significantly different from that of the standard sample, resulting in a large variation in the signal response value, thereby affecting the detection limit, quantitation limit, accuracy and Precision etc.

Method used

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  • Method for determining residual amount of three types of phenoxyalkanoic acid pesticides in tobaccos through extraction-purification synchronization method
  • Method for determining residual amount of three types of phenoxyalkanoic acid pesticides in tobaccos through extraction-purification synchronization method
  • Method for determining residual amount of three types of phenoxyalkanoic acid pesticides in tobaccos through extraction-purification synchronization method

Examples

Experimental program
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Effect test

example 1

[0030] 1. Instruments and reagents:

[0031] Pesticides: 2,4-D, 2,4,5-T and dicamba are standard products (purity greater than 98%); methanol and dichloromethane are of pesticide residue grade, and hydrochloric acid is of analytical grade.

[0032] Waters liquid chromatography-tandem quadrupole mass spectrometer; vortex oscillator (Labnet, USA); AE 163 electronic balance (sensitivity: 0.0001g) (Mettler, Switzerland).

[0033] 2. Sample handling:

[0034] 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 , vortex for 15 minutes. Pipette 1 mL of the lower organic phase, filter, and enter UPLC-MS / MS for detection;

[0035] 3. Prepare the standard working solution: Weigh 0.01 g of 2,4-D, 2,4,5-T and dicamba standard pesticides into different 10 mL volumetric flasks, and use CH 2 Cl 2 Dilute to constant volume to prepare a standard stock solution of 1000 μg / mL; pipette 100 μL of the abo...

example 2

[0039] 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 0.11 mg / kg.

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Abstract

The invention provides a method for determining the residual amount of three types of phenoxyalkanoic acid pesticides in tobaccos through an extraction-purification synchronization method. The methodis characterized by comprising the following steps: extracting a sample by utilizing a 0.5mol/L hydrochloric acid water solution; carrying out back extraction by utilizing dichloromethane; determiningthe residual amount of the pesticides including 2,4-D, 2,4,5-T and dicamba by utilizing an ultra performance liquid chromatography tandem mass spectrometry. According to the method provided by the invention, a standard working solution is prepared by utilizing a blank matrix and the influences on a matrix effect are overcome and the disadvantages of a sample treatment method in the prior art aremade up; a sample pre-treatment method and an instrument detection condition are optimized aiming at the tobacco sample; 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 does not need derivatization; 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 extraction-purification simultaneous method determination. 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 ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
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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