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Quick measurement method for fluxapyroxad residue in animal derived foods

A technology of flufenapyramide and animal origin, applied in a method field, can solve the problems of low sensitivity of anti-interference ability, limited effect, limited ability, etc., and achieve the effect of avoiding matrix interference, simple operation and high sensitivity

Inactive Publication Date: 2016-06-22
崔淑华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometer (GC-MS), and are generally equipped with negative chemical ion source (NCI). Now many types of pesticides contain electronegative groups, organochlorine and pseudo Most pyrethroid pesticide molecules contain strong electronegative groups such as -F, -Cl, -Br or -COO-; most organophosphorus pesticide molecules contain =S, -OR, -P, -O-, -Cl, or -P=O and other electronegative groups; and most of the new pesticides developed in recent years contain -F groups. Therefore, the use of GC-NCI-MS can facilitate the multi-residue analysis of various pesticides. Compared with MS, it can obta

Method used

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  • Quick measurement method for fluxapyroxad residue in animal derived foods
  • Quick measurement method for fluxapyroxad residue in animal derived foods
  • Quick measurement method for fluxapyroxad residue in animal derived foods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Detection of flufenapyramide residues in pork

[0033] (1) Sample pretreatment

[0034] extract

[0035] Weigh 5g of fully mixed pork sample into a 50mL centrifuge tube, add 10mL of water to resuscitate for 30min, then accurately add 20mL of acetonitrile solution, shake and extract for 20min, ultrasonically extract for 5min, add 3g of anhydrous magnesium sulfate and 2g of sodium chloride, vortex After 1min, centrifuge at 7000r / min for 5min and wait for purification.

[0036] purify

[0037] Add 4mL of water to the purification tube equipped with enhanced lipid removal product EMR, vortex to fully activate, pipette 6mL sample extract into the activated EMR purification tube, vortex for 1min, and then centrifuge at 7000r / min for 5min , transfer all the supernatant to a centrifuge tube filled with anhydrous magnesium sulfate and sodium chloride for salting out, after vortex centrifugation, pipette 4mL of the supernatant, concentrate to dryness, and use a volu...

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Abstract

The invention discloses a quick measurement method for fluxapyroxad residue in animal derived foods. The method is mainly used for measuring the content of residual fluxapyroxad in the animal derived foods with high fat content. The method comprises the following steps: homogeneously extracting residual fluxapyroxad from a sample using acetonitrile; performing EMR (enhanced matrix removal) matrix dispersion purification as well as reverse-extraction tube extraction and concentration on the extract; performing GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) detection; establishing a corrected standard work curve using a blank matrix solution without the pesticide to be detected; and quantifying by an external standard method. With average recovery rate of 86.7-93.8%, average RSD (relative standard deviation) of 6.0-7.8% and detection limit lower than 2.46mug/kg, the method has the advantages of simplicity and quickness in detection, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and qualitative and quantitative accuracies and can meet the technical requirements on the safety detection of corresponding products in countries including America, Europe and Japan and provide powerful technical support to guarantee the food safety for national people and the sound development of export trade.

Description

technical field [0001] The invention relates to a rapid determination method for flufenapyroxamide residues in animal-derived foods, more specifically, qualitative and quantitative determination of pork, beef and mutton by gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) The invention discloses a method for residual flufenapyramide content in animal-derived foods with high fat content such as chicken, chicken and other animal muscles and products, which belongs to the technical field of determination of pesticide residues. 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....

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/062
Inventor 崔淑华
Owner 崔淑华
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