Method for rapidly determining residual fenpyrazamine in animal-derived foods

Abstract

The invention discloses a rapid determination method for fenpyrazolone residues in animal-derived foods. The method is mainly used for determining the residual fenpyrazolone content in animal-derived foods with high fat content. Use acetonitrile to homogeneously extract the residual fenpyrazolone in the sample, and the extract solution is dispersed and purified by Enhanced Matrix Removal (EMR) matrix, extracted and concentrated by stripping tube, and then gas chromatography-negative chemical ion source- For mass spectrometry (GC‑NCI‑MS) detection, a blank matrix solution without the pesticide to be tested was used to establish a calibrated standard working curve, and the external standard method was used for quantification. The average recovery rate of this method is 90.4%-93.6%, the average relative standard deviation (RSD) is 5.8%-6.8%, and the detection limit is lower than 3.90 μg / kg. Strong characteristic, good repeatability, 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 fast determination method of pyrazolone residue in animal origin food, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure pork, beef, The invention relates to a method for residual fenpyrazolone content in animal-derived foods with high fat content such as mutton, chicken and other animal muscles and products, belonging to the technical field of determination of pesticide residues. Background technique [0002] Fenpyrazamine is a pyridine-based heterocyclic fungicide developed by Sumitomo Chemical Co., Ltd., which inhibits the pathogens of the ergosterol biosynthetic pathway, and shows effects on mycelial growth and spore germination and Inhibition of pollen tube growth. The CAS number is: 473798-59-3, the molecular formula is C 17 h 21 N 3 o 2 S, the molecular weight is 331.43, and the chemical structural formu...

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 fenpyrazolone residues in food and agricultural products

In addition, it is well known that the QuEChERS pretreatment technology has become the most widely used sample pretreatment method in the analysis of pesticide residues, but the QuEChERS method is mainly suitable for low-fat high-water substrates, such as most fruits and vegetables, in the face of high-fat content The capacity of the matrix is ​​limited, and it is generally necessary to add n-hexane degreasing, frozen sample extract degreasing and other steps, but the effect is limited

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