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Gas chromatography-mass spectrometer (GC-MS)/MS measuring method for 20 pesticide residues in tobaccos and tobacco products
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A technology for pesticide residues and tobacco products, applied to measuring devices, instruments, scientific instruments, etc.
Active Publication Date: 2013-01-09
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Shi Jie et al. used microwave-assisted extraction and GC-ECD detection method to simultaneously determine 17 organochlorine pesticides. The sensitivity is high and the detection limit is low, but the method is prone to false positives and misjudgment
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example 1
[0045] 1. Instruments and reagents:
[0046] 20 kinds of pesticides: Captafol, Demeton-O, Dimeform, Demeton-S, Octaphos, Zikewei, Diamon, Metolachlor, Webacil, Napropamide, Dimefoam Azole, ethyl acetofen, myclobutanil, rice blastin, clofenac, carbosulfan, bromfenphos, dicofen, carbosulfan, quizalofop-ethyl, internal standard: TPP, all are standard products; acetonitrile, acetone, toluene, all are chromatographic grade reagents; distilled water, meet the requirements of first-grade water in GB / T 6682.
[0047] American Thermo Fisher TSQ Quantum GC gas chromatography-triple quadrupole tandem mass spectrometer; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g); American Labnet VtexMixer VX200 oscillator; German Sigma high-speed refrigerated centrifuge.
[0048] 2. Sample handling:
[0049] Weigh about 2 g of sample, accurate to 0.01 g, into a 50 mL centrifuge tube with a cover, add 10 mL of water, shake until the sample is fully infiltrated by water, and then let...
example 2
[0060] As described in Example 1, another tobacco sample B was selected, and the contents of 20 pesticide targets in the sample were measured in Table 4.
[0061] serial number Chinese common name The content of pesticide target in the sample (ng / g) 1 Captafol — 2 Demeton-O — 3 Dimeform 8.2 4 Demeton-S — 5 Octaphos — 6 Kewei — 7 metolachlor 7.4 8 Herbicide 14.8 9 Napropamide 17.7 10 Uniconazole 79.8 11 Ethyl Fofofol 18.3 12 myclobutanil 74.6 13 Rice blast spirit — 14 Pyracityl — 15 carbosulfan — 16 Mianlong — 17 Bromophenylphosphine — 18 Dicofen — 19 Carbosulfan 19.2 20 quizalofop-ethyl 19.7
[0062] Note: "—" means not detected
example 3
[0064] As described in Example 1, another tobacco sample C was selected, and the contents of 20 pesticide targets in the sample were measured in Table 5.
[0065] serial number Chinese common name The content of pesticide target in the sample (ng / g) 1 Captafol — 2 Demeton-O — 3 Dimeform — 4 Demeton-S — 5 Octaphos — 6 Kewei — 7 metolachlor 5.5 8 Herbicide — 9 Napropamide — 10 Uniconazole 15.8 11 Ethyl Fofofol — 12 myclobutanil 11.1 13 Rice blast spirit — 14 Pyracityl — 15 carbosulfan — 16 Mianlong — 17 Bromophenylphosphine — 18 Dicofen — 19 Carbosulfan 19.3 20 quizalofop-ethyl —
[0066] Note: "—" means not detected
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Abstract
A gas chromatography-mass spectrometer (GC-MS) / MS measuring method for 20 pesticide residues in tobaccos and tobacco products is characterized by comprising adding acetonitrile and an internal standard substance after a to-be-measured sample is soaked by water, then performing vortex extraction and salting-out layering, adding toluene to perform liquid-liquid extraction, taking supernatant to perform dispersive solid-phase extraction (d-SPE), and using a GC-MS / MS method to perform measurement. The method has the advantages that the water is utilized to soak the sample, and extraction effects of organic solvent acetonitrile added later on on pesticide targets are improved; freezing treatment is performed in advance before anhydrous magnesium sulfate is added, so that thermal degradation of part of the targets caused by severe heat release of anhydrous magnesium sulfate in the dewatering process is avoided; toluene is added in the sample extract liquid after extraction salting-out, the obtained extract liquid has shallower color than when acetonitrile is independently used, and the effects of diluting the extract liquid and partially removing impurities for the extract liquid are achieved actually.
Description
technical field [0001] The invention belongs to the technical field of pesticide residue detection in tobacco and tobacco products, and mainly relates to captafol, demeton-O, chlordimeform, demeton-S, octamethylphos, Zikewei, Metron, metolachlor, webacid, napropamide, uniconazole, ethyl acetofen, myclobutanil, riceblastyl, clofenacyl, carbosulfan, bromfenphos, triclosan Determination techniques for 20 kinds of pesticide residues such as sulfone, carbosulfan, and quizalofop-p-ethyl. [0002] Background technique [0003] Pesticide residues refer to trace amounts of pesticides and their metabolites and degradation products that remain in the environment, crops, and organisms after pesticides are applied to crops. During the growth of tobacco seedlings and storage after picking, herbicides, plant growth regulators, insecticides, acaricides and fungicides are inevitably used. Simultaneously, as a kind of smoking food, tobacco has high safety requirements. Therefore, pesticide...
Claims
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 胡清源陈晓水唐纲岭侯宏卫边照阳杨飞张洪非
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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