GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of metrafenone in fruits and vegetables

Abstract

The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of metrafenone in fruits and vegetables. 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 dispersion and purification on an extraction solution with a matrix of ethylenediamine-N-propylsilane (PSA) and octadecylsilane bonded phase (C18), then performing 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 89.9%-94.9%, the average relative standard deviation (RSD) is 4.1%-6.2%, the detection limit is lower than 1.02mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, high sensitivity, 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 invention relates to a GC-NCI-MS method for determining the residual amount of metrafenone in fruits and vegetables, more specifically, it adopts gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure the residual amount of metrafenone in vegetables and fruits. The method for the content of residual metrafenone belongs to the technical field of determination of pesticide residues. Background technique [0002] Metrafenone (metrafenone, CAS 220899-03-6), 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 plant chemical protection. The trade name is Flexity, and its structural formula is: [0003] [0004] Metrafenone has been registered in the United Kingdom, the Netherlands and other countries since 2003. It has the fu...

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- The report of the NCI-MS detection method, therefore, it is of great significance to establish a gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection method for the qualitative and quantitative analysis of metrafenone residues in vegetables and fruits

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