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Pyrifluquinazon residue determination method

A determination method and technology of residues, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as toxicity, achieve good repeatability, ensure people's food safety, and avoid matrix interference

Active Publication Date: 2014-04-16
崔淑华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although Pyrifluquinazon has little effect on neurotoxicity and genotoxicity, it has toxic effects on testes, liver and blood pressure

Method used

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  • Pyrifluquinazon residue determination method
  • Pyrifluquinazon residue determination method
  • Pyrifluquinazon residue determination method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: the detection of Pyrifluquinazon residue in apple

[0041] (1) Sample pretreatment

[0042]Weigh 10.0 g of well-mixed apples into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, vortex for 1 min, and centrifuge at 5000 r / min for 5 min. After centrifugation, take 2mL of acetonitrile extract and transfer to a solution containing 300mg of anhydrous magnesium sulfate, 50mg of C 18 , 50mg PSA and 15mgCarb in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 3min. Take the supernatant and pass it through a 0.22 μm filter membrane, and wait for determination.

[0043] (2) Preparation of standard working solution

[0044] Weigh 10g apple blank sample, prepare blank matrix solution through the above pretreatment steps, dilute 100ng / mL standard solution with acetonitrile to 10ng / mL standard intermediate solution, and dilute standard...

Embodiment 2

[0077] Example 2: Detection of pyrifluquinazon residues in tea leaves

[0078] (1) Sample pretreatment

[0079] Weigh 2.0g of fully mixed tea into a 50mL centrifuge tube, add 5mL of water to revive for 30min, then accurately add 20mL of 1% acetic acid acetonitrile, extract homogeneously for 1min, add 3g of anhydrous magnesium sulfate, 2g of sodium acetate and 3mL of water, vortex After 1min, centrifuge at 5000r / min for 5min. After centrifugation, take 2mL of acetonitrile extract and transfer to a solution containing 300mg of anhydrous magnesium sulfate, 50mg of C 18 , 50mg PSA and 15mgCarb in a centrifuge tube, vortex for 1min, centrifuge at 5000r / min for 3min, pass through a 0.22μm filter membrane into a brown sampling vial, and wait for LC-MS / MS determination.

[0080] (2) Preparation of standard working solution

[0081] Weigh 2g tea blank sample, prepare blank matrix solution through the above pretreatment steps, use it to dilute and prepare 0.5, 1, 2, 5, 10, 20, 50ng / m...

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Abstract

The invention discloses a Pyrifluquinazon residue determination method. The method comprises the steps of homogenously extracting residual Pyrifluquinazon in a sample through acetonitrile or 1% acetic acid acetonitrile, dispersing and purifying an extracting solution through ethylenediamine-N-propyl silicane (PSA), octadecyl silicane bonded phase (C18) and graphitized carbon (Carb) substrate, implementing liquid chromatogram-tandem mass spectrum (LC-MS / MS) detection, establishing a correction standard curve through a blank matrix solution dilution standard, and quantifying through an external standard method. According to the determination method disclosed by the invention, average recovery rate is 85.3-92.0%, average relative standard deviation (RSD) is 3.5-6.1% and detection limit is lower than 0.38 mu g / kg, and the method has the advantages of simplicity and rapidness in operation, high sensitivity, good repeatability, and accuracy in qualitative and quantitative determination. The method can satisfy technical requirements of Korea, Japan, European Union and other countries on corresponding product safety detection, and provide powerful technical support for guaranteeing food safety of Chinese people and healthy development of export trade.

Description

technical field [0001] The present invention relates to a method for determining the residual amount of pyrifluquinazon, more specifically, a method for qualitatively and quantitatively measuring the residual pyrifluquinazon content in vegetables, fruits and tea leaves by using high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS), which belongs to pesticides Determination of residues technical field. Background technique [0002] Pyrifluquinazon is a new quinazoline insecticide with a bisamide structure invented by Japan Pesticide Company and jointly developed by Japan Combination Chemical Company. It is mainly used to control aphids, whiteflies and mealybugs on vegetables, fruit trees and tea. , leafhoppers, thrips and other piercing-sucking pests. The chemical name is 1-acetyl-3,4-dihydro-3-[(3-pyridylmethyl)amino]-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl ) ethyl]-2-(1H)-quinazolinone, the CAS accession number is 337458-27-2, and the structural for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 崔淑华汤志旭肖西志王英华王静王兴华
Owner 崔淑华
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