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Method for simultaneously determining residue of common herbicide in tobacco

A technology of herbicides and residues, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low detection efficiency, cumbersome operation, and long time consumption, so as to reduce procedures and preparations, reduce volatile volume, and improve stability Effect

Inactive Publication Date: 2017-08-15
贵阳海关综合技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing detection standards and literature cannot simultaneously determine the 15 herbicide residues in tobacco with the above-mentioned limited limits by one method, and there are problems such as low detection efficiency, cumbersome operation, and long time-consuming. Herbicide residue approach looms

Method used

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  • Method for simultaneously determining residue of common herbicide in tobacco
  • Method for simultaneously determining residue of common herbicide in tobacco
  • Method for simultaneously determining residue of common herbicide in tobacco

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0039] Embodiment 1: A kind of method of herbicide residue commonly used in measuring tobacco simultaneously is characterized in that: target substance in the tobacco sample is extracted through acidified acetonitrile, cleans up with florisil solid phase extraction small column, acetone / cyclohexane (volume ratio 3:7) mixed solution was eluted, and the eluate was concentrated and derivatized with trimethylsilyl diazomethane, and then detected by online gel permeation chromatography-gas chromatography-tandem mass spectrometry.

[0040] A method for simultaneously measuring the herbicide residues commonly used in tobacco, the method's concrete steps are as follows::

[0041] (1) Preparation of internal standard solution: prepare an acetone internal standard solution with a pretilachlor concentration of 10 μg / mL;

[0042] (2) Derivatizing agent: 2 mol / L trimethylsilylated diazomethane n-hexane solution;

[0043] (3) Extraction of herbicide targets: Weigh 2.00 g of dried and groun...

Embodiment 2

[0056] Embodiment 2: the detection of 16 kinds of herbicide residues in the tobacco sample

[0057] 1. Instruments and reagents:

[0058] Online gel permeation chromatography-gas chromatography-tandem mass spectrometry system (Online GPCGCMS / MS system) (Shimadzu Corporation), including SIL20ADvp autosampler, ShodexEV200A gel permeation chromatography column, CEO20ASvp column thermostat, SPD20Avp UV detection Instrument, QP2010Plus gas chromatograph, TQ8040 mass spectrometer, PTV2010 large volume sampler, X-22R high-speed refrigerated centrifuge (Allegra, USA), vortex shaker (TAIBOYS, USA), AL204 analytical balance (Mettler, USA ), TurboVap II nitrogen blowing instrument (Sweden Biotage Company).

[0059] Acetonitrile (chromatographically pure), acetone (chromatographically pure), cyclohexane (chromatographically pure), sodium chloride (pesticide residue grade), acetic acid (chromatographically pure); experimental water is Milipore-Q ultrapure water; derivatizer: 2 mol / L trim...

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Abstract

The invention discloses a method for simultaneously determining the residue of a common herbicide in tobacco. The method comprises the following steps: using acidified acetonitrile for extracting a target object in a tobacco sample; using a florisil solid-phase extracting column for purifying; eluting with a mixed solution of acetone / cyclohexane at a volume ratio of 3:7; concentrating the eluent and then adopting trimethyl silanized diazomethane for derivatizing; and utilizing an online gel permeation chromatography-gas chromatography-tandem mass spectrum combined instrument for detecting. Compared with a standard method, the method has the advantages that the detection indexes of four standard methods are combined, dacthal is added, the detection efficiency is obviously increased, the sensitivity is higher, the anti-interference capacity is higher, and the high recovery rate of the sample and the excellent reproducibility are greatly guaranteed.

Description

technical field [0001] The invention belongs to the field of detection of pesticide residues in tobacco, and relates to the detection technology of pesticide residues in tobacco, in particular to a method for determining the residues of herbicides commonly used in tobacco, specifically detecting dicamba, 2,4-D, trifluralin, fluorine Laxam, 2,4,5-T, Clomazone, Dibenzamide, Alachlor, Napropamide, Dimethoxol, S-Butyl, Propylene, Pendimethalin, Fluorine The residues of 16 kinds of herbicides including amine, fenfen and fluazifop-ethyl were studied. Background technique [0002] Tobacco is an important economic crop in my country. In recent years, the application of herbicides has greatly reduced labor intensity, effectively improved agricultural production efficiency, and played a positive role in the yield and quality of tobacco leaves. With the expansion of the use of herbicides, the harm caused by herbicide residues to human health and the environment has attracted more and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/062G01N2030/067
Inventor 王兴宁曹桂红
Owner 贵阳海关综合技术中心
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