A kind of assay method of pyrifluquinazon residue

Abstract

The invention discloses a determination method for Pyrifluquinazon residual quantity. The method is mainly used for determining the content of residual Pyrifluquinazon in complex matrix food and agricultural products such as cereal grains and animal derived foods. Homogeneous extraction of residual Pyrifluquinazon in samples is carried out by using acetonitrile or an acetonitrile solution containing 1% of acetic acid, after purification and concentration with a C18 / PSA solid-phase extraction column, gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection is carried out, a corrected standard curve is established by adopting a blank substrate solution which does not contain a pesticide to be tested, and quantization is carried out by an external standard method. According to the method, the average recovery rate is 75.1%-80.2%, the average relative standard deviation (RSD) is 4.8%-8.0%, the detection limit is lower than 2.77 microg / kg, and the determination method has the advantages of easiness, convenience and quickness in operation, good impurity removal effect, high sensitivity, marked characteristics, good repeatability, and accurate qualification and quantization. The determination method can meet the technical requirement of countries such as Japan, European Union and South Korea for 0.01mg / kg residue limit in corresponding food safety testing, namely 'uniform standard', so as to provide powerful technical support for guaranteeing the food safety of Chinese people and the healthy development of export trade.

Description

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

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. Pyrifluquinazon is an electronegative compound, but so far there is no GC-NCI-MS detection of Pyrifluquinazon residues in vegetables and fruits In the report of the method, 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 chemical ion source-mass spectrometry (GC-NCI-MS) method for the qualitative and quantitative analysis of Pyrifluquinazon residues in grains and foods of animal origin is of great significance

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