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Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products

A technology for pesticide residues and phenoxycarboxylic acids, applied in measuring devices, instruments, scientific instruments, etc.

Active Publication Date: 2013-01-02
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Determination of phenoxyacetic acid herbicides in tobacco by liquid chromatography-tandem mass spectrometry has not been reported

Method used

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  • Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products
  • Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products
  • Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] 1. Instruments and reagents:

[0035] Pesticides: 2,4-D, 2,4,5-T and dicamba are all standard products; acetonitrile and acetic acid are all pesticide residue grades.

[0036] API 4000 quadrupole tandem mass spectrometer; vortex oscillator (Labnet, USA); Sigma 3-30K centrifuge (Sigma, Germany); AE 163 electronic balance (sensitivity: 0.0001g) and AE 166 electronic balance (sensitivity : 0.01g) (Mettler, Switzerland).

[0037] 2. Sample handling:

[0038] Accurately weigh 2 g of sample (accurate to 0.01 g) into a 50 mL capped centrifuge tube, add 10 mL of water, and shake until the sample is fully wetted by water. After standing still for 10 min, pipette 10 mL of acetonitrile into the centrifuge tube, add 200 μL of acetic acid, then place the centrifuge tube on a vortex mixer and vibrate at 2000 rpm for 1 min. Keep the centrifuge tube at -18°C for 10 min, then add 4 g of anhydrous magnesium sulfate and 1 g of sodium chloride, 1 g of sodium citrate and 0.5 g of sodiu...

example 2

[0044] Example 2: According to the method described in Example 1, another tobacco leaf sample was selected, and the residual amounts of 2, 4 drops and dicamba in the sample were measured to be 0.12 μg / g and 0.18 μg / g, respectively.

example 3

[0045] Example 3: According to the method described in Example 1, another tobacco leaf sample was selected, and the 2,4,5-T content in the sample was measured to be 0.22 μg / g.

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Abstract

The invention discloses a method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products. The method is characterized by comprising the following steps of: digesting a sample by using acetonitrile; adding anhydrous magnesium sulfate, sodium chloride, sodium citrate and sodium hydrogen citrate to oscillate for layering; and subsequently, performing dispersive solid-phase extraction, and directly measuring the pesticide residues of 2,4-drop, 2,4,5-mucus and dicamba in the tobacco and tobacco products through liquid chromatogram-tandem mass spectrometry. According to the method, the defects of the sample treatment method in the prior art are overcome, and the sample pretreatment method and the instrument detection conditions are optimized aiming at the tobacco products; and compared with the prior art, the method has the beneficial effects that the sample pretreatment process is simple and rapid, derivatization is not required, and the method has the advantages that operation is accurate, sensitivity is high and repeatability is high.

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 measurement techniques. Background technique [0002] Tobacco is a smoking food, and its pesticide residue problem has become an important part of smoking safety issues. The pesticide residue index of tobacco and tobacco products is an important content in the quality control of tobacco products in various countries, and has become an important part of tobacco leaf evaluation and selection in the international market. It is an important factor in the purchase of tobacco and an important content of commodity inspection in the international trade of tobacco. Phenoxyacetic acid substances are the earliest herbicides developed and put into use. Because of its low ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杨飞唐纲岭边照阳范子彦李中皓张洪非李雪庞永强胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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