Method for measuring pesticide residue of six kinds of dinitroaniline in tobacco and tobacco products
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A technology for pesticide residues and dinitroaniline, which is applied to measuring devices, instruments, scientific instruments, etc., can solve the problems of complicated operation steps and high toxicity, and achieve the effects of shortening the pre-extraction treatment time, easy operation and reducing pollution.
Inactive Publication Date: 2009-03-25
ZHENGZHOU TOBACCO RES INST OF CNTC
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GB/T 13595-2004 [National Standard of the People's Republic of China GB/T 13596-2004 Tobacco and Tobacco Products Determination of Pyrethroid Insecticides, Organophosphorus Insecticides, and Nitrogenous Pesticide Residues] stipulates that tobacco and tobacco products The determination method of 4 kinds of dinitroaniline pesticides, such as flubenzamine, buddingin, propramid and pendimethalin, provides a good analytical basis for the detection of this kind of pesticide residues, but the method uses acetone High-speed homogenate extraction extracts pesticide residues in tobacco, liquid/liquid partitioning with ethyl acetate and cyclohexane, gel permeation chromatography and silica gel column chromatography purification, gas chromatography (ECD detector) and gas chromatography/mass spectrometry method, the operation steps are relatively complicated, and a large amount of organic solvents are used, which is highly toxic to the experimenter
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example 1
[0031] 1. Instruments and reagents:
[0032] Pesticides: buddingin, flumetriamine, propramid, pendimethalin, butafluralin and trifluralin, internal standard: mirex, all standard; anhydrous Na 2 SO 4 , analytically pure; n-hexane (pesticide residue grade); Florisil (Florisil, 60 mesh-100 mesh, pesticide residue grade).
[0033] Agilent 6890N gas chromatograph equipped with ECD detector; ASE-200 accelerated solvent extractor (Dionex, USA); AE 163 electronic balance (sensitivity: 0.0001g) and AE166 electronic balance (sensitivity: 0.01g) (Swiss Mettler company).
[0034] 2. Sample processing:
[0035] Anhydrous sodium sulfate: Bake in a muffle furnace at 550°C for 4 hours before use.
[0036] Florisil: Burn Florisil in a muffle furnace at 550°C for 5h, cool it in a desiccator without desiccant, add 5% (mass fraction) of water, mix well, and place in a closed Equilibrate in a glass container for at least 48h.
[0037] Accurately weigh 5g of tobacco powder (accurate to 0.01g)...
example 2
[0043] As described in Example 1, another tobacco leaf sample was selected, and the residual amounts of protopazin and flumethamine in the sample were measured to be 0.86 μg / g and 0.13 μg / g, respectively.
example 3
[0045] As described in Example 1, another tobacco leaf sample was selected, and the residual amounts of propamethalin and pendimethalin in the sample were measured to be 0.77 μg / g and 4.02 μg / g, respectively.
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Abstract
The invention belongs to the technical field of physicochemical testing of residual pesticide in tobacco and a tobacco product and in particular to a method for mensurating the residual amounts of six classes of dinitraniline pesticides, The method is to extract residual pesticides in an accelerated solvent extraction instrument (ASE), and use a gas chromatograph (matched with electron capture detector (ECD) to directly mensurate the residual amounts of six classes of the dinitraniline pesticides in the tobacco and the tobacco product, namely, butralin, flumetralin, isopropalin, pendimethalin, benfluralin and trifluralin. The method overcomes the disadvantages of a sample treatment method in the prior art and optimizes a sample pretreatment method and the instrument detecting conditions aiming at a tobacco sample. Compared with the prior art, the method has the advantages of simple pretreatment process, reduction of the interference of pigment and other impurities in the tobacco, high automation degree of the whole operation, accurate 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 tobacco and tobacco products, including six types of acetaminophen, flubenzamine, propralacin, pendimethalin, butadifluralin and trifluralin, etc. A kind of assay technology of dinitroaniline pesticide residues, specifically a kind of extraction of pesticide residues in accelerated solvent extractor (ASE), direct determination of tobacco and tobacco products with gas chromatography (with electron capture detector (ECD)) method for the residues of six dinitroaniline pesticides. 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 par...
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