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High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products

A technology of amide herbicides and high performance liquid chromatography, which is applied to measuring devices, instruments, scientific instruments, etc.

Inactive Publication Date: 2013-09-18
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method needs to consume a large amount of solvent, and the method is cumbersome and time-consuming

Method used

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  • High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products
  • High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products
  • High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0027] 1. Instruments and reagents:

[0028] All three pesticides are standard products; acetonitrile and formic acid are all pesticide residue grades.

[0029] 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).

[0030] 2. Sample handling:

[0031] 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 for 10 min, add 10 mL of acetonitrile and 50 μL of internal standard (chlorazophos, 20 μg / mL) into the centrifuge tube, then place the centrifuge tube on a vortex mixer and vibrate at 2000 rpm for 1 min. Place the centrifuge tube at 0 °C for 10 min, then add the Agilent SampliQ QuEChERS EN extraction kit (Agilent 5982-5650) to the centrifuge tube, and immediately...

example 2

[0038] As described in Example 1, another tobacco leaf sample was selected, and the residual amount of napropamide in the sample was measured to be 0.05 μg / g.

example 3

[0040] As described in Example 1, another tobacco leaf sample was selected, and the content of alachlor in the sample was measured to be 0.09 μg / g.

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Abstract

The invention relates to a high performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides (i.e., alachlor, metolachlor and napropamide) in tobacco and tobacco products, which belongs to the technical filed of physical and chemical inspection of pesticide residue in the tobacco and tobacco products. The high performance liquid chromatography-tandem mass spectrometry measuring method is characterized by being the method which is used for directly extracting the pesticide residue by a substrate dispersion solid-phase extraction method to directly measure the pesticide residue in the tobacco and tobacco products by virtue of chromatography-tandem mass spectrometry. The high performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products disclosed by the invention can be used for overcoming the defects of the sample treatment method in the prior art, and optimizing the sample pre-treatment method and the apparatus detection condition for the tobacco sample. Moreover, compared with the prior art, the method disclosed by the invention has the excellent effects that the sample pre-treatment process of the method is simple and quick, capable of reducing the interferences of the impurities including pigment and the like in the tobacco, and provided with the advantages of being accurate to operate, high in flexibility and good in 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 the measurement technology of amide herbicide residues in tobacco and tobacco products. Specifically, samples are extracted with acetonitrile, and then anhydrous magnesium sulfate is added. Vibration with sodium chloride etc. promotes its layering, followed by dispersive solid-phase extraction and liquid chromatography-tandem mass spectrometry to directly determine the residues of three amide herbicides in tobacco and tobacco products. Background technique [0002] Amide herbicides are a class of highly efficient and highly selective contact herbicides developed in the 1960s. It has a strong anti-virus effect on a variety of grass dicotyledonous plants, and is mainly used to control the young shoots of annual grass weeds. In vivo experiments in rats have shown that amide herbicides can be further...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 杨飞唐纲岭边照阳范子彦李中皓张洪非庞永强胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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