GC-NIC-MS measurement method for penflufen residual amount

Abstract

The invention discloses a GC-NCI-MS method for determining the residual amount of flufenapyroxamide, which is mainly used for measuring the residual flufenapyroxystrobale content in complex matrix food and agricultural products such as grains and animal-derived foods. Use acetonitrile or an acetonitrile solution containing 1% acetic acid to homogeneously extract the residual flufenapyramide in the sample, C 18 After purification and concentration of the / PSA solid phase extraction column, gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection, a calibration standard working curve is established using a blank matrix solution that does not contain the pesticide to be tested, and the external standard method is used for quantification. The average recovery rate of this method is 88.9%-104.7%, the average relative standard deviation (RSD) is 4.2%-7.5%, and the detection limit is lower than 1.09 μg / kg. Strong characteristics, good repeatability, and accurate qualitative and quantitative advantages. It can meet the technical requirements of the United States, the European Union, Japan and other countries for corresponding product safety testing, and provide strong technical support for ensuring the food safety of our people and the healthy development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of GC-NCI-MS determination method of flufenapyramide residual amount, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure grain, pork, The invention relates to a method for residual flufenapyroxamide content in animal and plant-derived foods with complex matrices such as beef, mutton, chicken and other animal muscles and products, and 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, metha...

AI Technical Summary

Problems solved by technology

Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometers (GC-MS), and are generally equipped with negative chemical ion sources (NCI). Now many types of pesticides contain electronegative groups, organochlorines and pseudo Pyrethrin pesticide molecules mostly contain strong electronegative groups such as -F, -Cl, -Br or -COO-; organophosphorus pesticide molecules mostly 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 obtain better anti-interference ability, lower sensitivity and better selectivity, but so far there is no report on the GC-NCI-MS detection method of flufenapyroxamide residues in food and agricultural products. Pyraclostrobin is an electronegative compound. Due to the complex matrix of food and agricultural products such as grains and animal-derived foods, it is necessary to establish a sample pretreatment method and instrument analysis conditions with good purification effects to meet the detection requirements. Therefore, the establishment of gas chromatography-negative The detection method of chemical ion source-mass spectrometry (GC-NCI-MS) is of great significance for the qualitative and quantitative analysis of flufenapyramide residues in grains and animal-derived foods

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