GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing dinitroaniline pesticide residue in tobacco and tobacco product
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A technology of dinitroaniline and tobacco products, applied in the field of pesticide residue detection
Active Publication Date: 2013-09-11
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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The use of gas chromatography-tandem mass spectrometry (GC-MS / MS) for the separate analysis of dinitroaniline pesticide residues has not been reported
Method used
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example 1
[0040] 1. Instruments and reagents:
[0041] Dinitroaniline pesticides: butylfluralin, secbutaline, trifluralin, isopramid, pendimethalin, trifluralin, internal standard: TPP, all standard; acetonitrile, acetone, n-hexane , are 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 working solution, and place on a vortex mixer for 1 min at ...
example 2
[0058] As described in Example 1, another tobacco sample B was selected, and the content of the target dinitroaniline pesticides in the sample was measured in Table 4.
[0059] serial number Chinese common name The content of pesticide target in the sample (μg / g) 1 Butaflurane —— 2 Zhong Dingling 0.06 3 flumetriamine —— 4 Isoprofen —— 5 Pendimethalin 0.19 6 Trifluralin ——
[0060] Note: "—" means not detected
example 3
[0062] As described in Example 1, another tobacco sample C was selected, and the contents of the target dinitroaniline pesticides in the sample were measured in Table 5.
[0063] serial number Chinese common name The content of pesticide target in the sample (μg / g) 1 Butaflurane —— 2 Zhong Dingling 0.03 3 flumetriamine 2.70 4 Isoprofen —— 5 Pendimethalin —— 6 Trifluralin ——
[0064] 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 dinitroaniline 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 omits a purification step of substrate d-SPE (dispersive solid phase extraction); and instead, the acetonitrile extracting solution is taken, and liquid-liquid extraction and secondary salting-out are performed by using the n-hexane and the sodium chloride water solution, so that the polar coextraction substrate in the supernatant is greatly reduced. By using GC-MS / MS having high sensitivity and high interference rejection, the detection limit of a target substance can be greatly reduced, and the advantages of high sensitivity and favorable repetitiveness are achieved.
Description
[0001] technical field [0002] The invention belongs to the technical field of pesticide residue detection in tobacco and tobacco products, and mainly relates to the detection technology of nitro-type pesticide residues in tobacco and tobacco products. [0003] Background technique [0004] According to the chemical structure, organic pesticides mainly include organophosphorus, organochlorine, pyrethroids, carbamates, organic nitrogen (including amides and nitros), etc. Among them, dinitroaniline pesticides are also important indicators for the detection of pesticide residues in tobacco, and the detection rate of representative pesticide residues such as pendimethalin is relatively high. [0005] 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 g...
Claims
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 边照阳陈晓水陈再根唐纲岭杨飞刘珊珊李中皓刘洋张洪非胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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