GC-MS/MS method for determining fluxapyroxad residues in fruits and vegetables

A technology for mesofluoxamid, fruits and vegetables, applied in the field of pesticide residue determination, can solve the problems of high price, long system and the like, and achieve the effects of simple operation, good repeatability and ensuring people's food safety.

Inactive Publication Date: 2016-06-29
崔淑华
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At this stage, there are few studies on the determination of flufenapyroxamide residues. The reported detection methods are mainly the detection methods of flufenapyroxamide residues in vegetables and fruits. These detection methods are all based on liquid chromatography tandem mass spectrometry (LC-MS / MS) is a detection method for the determination of flufenapyramide residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. However, due to its high price, many testing institutions and enterprises Or the scientific research institute has not configured this instrument or the number of equipment is small. Since different compounds are detected by LC-MS / MS, different mobile phases or chromatographic columns need to be used, which requires constant replacement of chromatographic columns and mobile phases and takes a long time. The time to balance the system restricts the application of LC-MS / MS to some extent
The use of gas chromatography-tandem mass spectrometry (GC-MS / MS) to analyze pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, high sensitivity, and strong selectivity. It can achieve multi-residue analysis of hundreds of pesticides, but so far no food and agricultural products The report of the GC-MS / MS detection method for the residues of flufenapyramide in vegetables and fruits, so the GC-MS / MS that is simple, fast, accurate, durable, and can accurately qualitatively and quantitatively analyze the residues of flufenapyramide in vegetables and fruits has been established. The detection method is of great significance

Method used

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  • GC-MS/MS method for determining fluxapyroxad residues in fruits and vegetables
  • GC-MS/MS method for determining fluxapyroxad residues in fruits and vegetables
  • GC-MS/MS method for determining fluxapyroxad residues in fruits and vegetables

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Detection of Flufenapyr residues in apples

[0035] (1) Sample pretreatment

[0036] Weigh 10.0 g of well-mixed apples into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, vortex for 1 min, and centrifuge at 7000 r / min for 5 min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 1mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly, pass through the membrane, and transfer it to the sample bottle for GC- MS / MS determination.

[0037] (2) Preparation of standard working solution

[0038] Accurately weigh 25±0.1mg of the standard produc...

Embodiment 2

[0066] Example 2: Detection of Flufenapyr residues in cucumber

[0067] (1) Sample pretreatment

[0068] Weigh 10.0 g of well-mixed cucumber into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate, 2 g of sodium acetate and 2 mL of water, vortex for 1 min, Centrifuge at 7000r / min for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 1mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix well, then transfer it to an injection bottle for GC-MS / MS determination.

[0069] (2) Preparation of standard working solution

[0070] Dilute the 1000 μg / mL stan...

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Abstract

The invention discloses a GC-MS/MS method for determining fluxapyroxad residues in fruits and vegetables. According to the method, acetonitrile or an acetonitrile solution containing 1% acetic acid are adopted to homogeneously extract the residual fluxapyroxad in a sample, the extracting solution is subjected to matrix dispersion and purification of ethylenediamine-N-propyl silane (PSA) and an octadecyl silane bonded phase (C18), then gas chromatography-tandem mass spectrometry (GC-MS/MS) detection is performed, a blank matrix solution containing no pesticide to be detected is adopted to establish a standard working curve for correction, and quantification is performed by adopting an external standard method. The average recovery rate of the method is 86.0%-96.0%, the average relative standard deviation (RSD) of the method is 3.5%-7.1%, the detection limit of the method reaches 0.064 micrograms/kilogram or below, and the method has the advantages of being simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualititation and quantification, can meet the technical requirements for corresponding product safety detection of the United States, European Union, Japan and other countries and provides a powerful technical support for ensuring the people's food safety and healthy development of the abroad export trade of our country.

Description

technical field [0001] The present invention relates to a GC-MS / MS method for determining flufenapyramide residues in fruits and vegetables, more specifically, using gas chromatography-tandem mass spectrometry (GC-MS / MS) to qualitatively and quantitatively measure flufenapyrazole residues in vegetables and fruits A method for amide content belongs to the technical field of pesticide residue determination. Background technique [0002] Fluxapyroxad is a succinate dehydrogenase inhibitor fungicide developed by BASF. Chemical name: 3-difluoromethyl-1-methyl-N-(3',4',5'-trifluorobiphenyl-2-yl)-1H-pyrazole-4-carboxamide; molecular formula: C18H12F5N3O ; Relative molecular mass: 381.3; Melting point: 157°C; Relative density: 1.42. Solubility in solvents (g / L, 20°C): acetone > 250, acetonitrile 168, ethyl acetate 123, methanol 53.4, toluene 20.0. The chemical structural formula of flufenapyroxamide is as follows: [0003] [0004] Fluxapyroxad has the advantages of high e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N27/62
CPCG01N27/62G01N30/02G01N30/06G01N2030/025
Inventor 崔淑华
Owner 崔淑华
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