A kind of assay method of metrafenone residue

Abstract

The invention discloses a method for determining residual amount of metrafenone. The method is mainly used for determining the residual amount of metrafenone in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual metrafenone in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 83.9%-90.1%, the average relative standard deviation (RSD) is 4.0%-5.8%, the detection limit is lower than 0.67mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirements on safety detection of corresponding products in European Union, United States, South Korea, Japan and other countries can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.

Description

technical field [0001] The present invention relates to a kind of determination method of metrafenone residual amount, more specifically adopts gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure grain, pork, beef, mutton, chicken, etc. The invention relates to a method for residual metrafenone content in animal and plant-derived foods with complex matrices such as animal muscles and products, and belongs to the technical field of determination of pesticide residues. Background technique [0002] Metrafenone (metrafenone, CAS220899-03-6), the chemical name is (3-bromo-6-methoxy-2-methylphenyl)-(2,3,4-trimethoxy-6-methyl Phenyl) ketone is a novel benzophenone-type novel fungicide developed by BASF. It is a brand-new active ingredient in the field of phytochemical protection. The trade name is Flexity, and its structural formula is: [0003] [0004] Metrafenone has been registered in the United Kingdom,...

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. Metrafenone is an electronegative compound, but so far no GC- According to the report of the NCI-MS detection 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 chemistry Ion source-mass spectrometry (GC-NCI-MS) is of great significance for the qualitative and quantitative analysis of metrafenone residues in grains and animal-derived foods

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