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Method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables

A technology for flufenapyridine, fruits and vegetables, applied in the field of determination of pesticide residues, can solve the problems of high price and long system, and achieve the effect of simple operation, good repeatability and high sensitivity

Inactive Publication Date: 2016-04-20
崔淑华
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there are few studies on the determination methods of flufenadine residues, and the detection methods reported are mainly the detection methods of flufenadine 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 flufenapyridine residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of quickness, 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 flufenapyridine residues in the medium, so the establishment of a simple, fast, accurate, durable, accurate qualitative and quantitative analysis of the GC-MS / MS of the fluoxazone residues in vegetables and fruits The detection method is of great significance

Method used

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  • Method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables
  • Method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables
  • Method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables

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Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: the detection of flufenazine residues in apples

[0037] (1) Sample pretreatment

[0038] 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.

[0039] (2) Preparation of standard working solution

[0040] Accurately weigh 25±0.1mg of the standar...

Embodiment 2

[0068] Example 2: Detection of flufenapyridine residues in cucumber

[0069] (1) Sample pretreatment

[0070] 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.

[0071] (2) Preparation of standard working solution

[0072] Dilute the 1000 μg / mL...

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Abstract

The invention discloses a method for GC-MS / MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables. Penflufen remains in a sample is extracted by acetonitrile or an acetonitrile solution containing 1% acetic acid, the extracting solution is dispersed and purified by an ethylenediamine-N-propylsilane (PSA) and octadecylsilan bonded phase (C18) substrate, GC-MS / MS detection is performed, a corrected standard work curve is built by adopting a blank substrate solution without to-be-detected pesticide, and quantification is performed with an external standard method. The method has the average recovery rate being 84.3%-90.6%, the average relative standard deviation (RSD) being 5.0%-8.0%, and the detection limit lower than 0.032 microgram / kilogram, and has the advantages of simple operation, rapidness, high sensitivity, good repeatability, high qualitative and quantitative precision, thereby meeting the technical requirements for safety detection of corresponding products in the USA, EU, Japan, and other countries, and providing strong technical support for ensuring Chinese food safety and export abroad trade healthy development.

Description

technical field [0001] The invention relates to a GC-MS / MS method for determining the residues of flufenpyridine in fruits and vegetables, more specifically, the qualitative and quantitative determination of flufenpyridine residues in vegetables and fruits by gas chromatography tandem mass spectrometry (GC-MS / MS) A method for aniline content belongs to the technical field of pesticide residue determination. Background technique [0002] Fenflufen is a succinate dehydrogenase inhibitor fungicide developed by BASF, common name: penflufen; test code: BYF14182; chemical name: N-[2-(1,3-dimethylbutyl) Phenyl]-5-fluoro-1,3-dimethyl-1H-pyrazole-4-carboxamide; appearance: off-white powdery solid; melting point: 111°C; boiling point: decomposes before boiling point; decomposition temperature: 320°C; Vapor pressure: 1.2×10 -6 Pa(25℃); partition coefficient: KowlogP=3.3(20℃, pH=7); Henry constant: 1.05×10 -5 Pa·m 3 • mol-1 (25°C). Solubility: The solubility in water is 10.9mg / L (2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 崔淑华范昆
Owner 崔淑华
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