GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product
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A technology for pyrethroid and tobacco products, which is applied in the field of determination of pyrethroid pesticide residues
Active Publication Date: 2013-09-11
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Gas chromatography-tandem mass spectrometry (GC-MS / MS) has not been used alone for the detection and analysis of pyrethroid pesticides
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example 1
[0040] 1. Instruments and reagents:
[0041] Pyrethroid pesticides: bifenthrin, cyfluthrin, cyhalothrin, cypermethrin, deltamethrin, fenvalerate, flucyvalerate, permethrin (cis), permethrin (trans ), tefluthrin, internal standard: TPP, all standard; acetonitrile, acetone, n-hexane, all chromatographic grade reagents; distilled water, in line with the requirements of first-grade water in GB / T 6682.
[0042] 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.
[0043] 2. Sample handling:
[0044] 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 stand for 10 min. Pipette 10 mL of acetonitrile into a centrifuge tube, add 100 μL of internal standard wo...
example 2
[0059] As described in Example 1, another tobacco sample B was selected, and the contents of pyrethroid pesticide targets in the sample were measured in Table 4.
[0060] Table 4 Detection results of pesticide targets in sample B
[0061] serial number Chinese common name Content of pesticide target in the sample (μg / g) 1 Bifenthrin —— 2 Cyfluthrin —— 3 Cyhalothrin —— 4 Cypermethrin —— 5 deltamethrin —— 6 Fenvalerate 0.02 7 flucyvalerate —— 8 Permethrin (cis) —— 9 Permethrin (trans) —— 10 Tefluthrin ——
[0062] Note: "—" means not detected
example 3
[0064] As described in Example 1, another tobacco sample C was selected, and the contents of pyrethroid pesticide targets in the sample were measured in Table 5.
[0065] table 5 Detection results of pesticide targets in sample C
[0066] serial number Chinese common name Content of pesticide target in the sample (μg / g) 1 Bifenthrin —— 2 Cyfluthrin —— 3 Cyhalothrin 0.03 4 Cypermethrin —— 5 deltamethrin —— 6 Fenvalerate 1.32 7 flucyvalerate —— 8 Permethrin (cis) —— 9 Permethrin (trans) —— 10 Tefluthrin ——
[0067] Note: "—" means not detected
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Abstract
The invention relates to a GC-MS / MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and a tobacco product, which is characterized by comprising the following steps: drenching a sample with water, and adding acetonitrile and an internal standard substance; performing vortex extraction and salting-out stratification, and performing secondary salting-out and liquid-liquid extraction with a sodium chloride water solution and n-hexane; and taking the n-hexane supernatant, and determining according to a GC-MS / MS method. The method provided by the invention simplifies the existing sample treatment method, provides a cleaner on-machine solution, and reduces the maintenance of instruments in the operating process. The sample pretreatment process of the method provided by the invention employs the step of drenching the sample with water in the existing method to improve the extraction effect of the acetonitrile on a pesticide target substance, and simultaneously omits the step of putting into a refrigerator before adding into a salting-out package. Inspection discovers that most of pyrethroid pesticides are thermostable, so that the pyrethroid pesticides can not be degraded due to heat release caused by the combination of anhydrous magnesium sulfate and water, thus saving the operating time herein.
Description
technical field [0001] The invention belongs to the technical field of pesticide residue detection in tobacco and tobacco products, and mainly relates to the detection technology of pyrethroid pesticide residues in tobacco and tobacco products. [0002] Background technique [0003] Pyrethroid pesticides are broad-spectrum insecticides that can control a variety of pests. Their insecticidal ability is stronger than that of organochlorine and organophosphorus. Therefore, their dosage is small, their concentration is low, and they are less harmful to humans and animals. But because of this, the use of pyrethroid pesticides is more extensive, and its detection rate is also higher. [0004] 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 regul...
Claims
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 杨飞陈晓水边照阳唐纲岭刘珊珊陈再根刘洋张洪非李中皓胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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