GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for residual quantity of cyenopyrafen in fruits and vegetables

Abstract

The invention discloses a GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for the residual quantity of cyenopyrafen in fruits and vegetables. The GC-NCI-MS detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual cyenopyrafen in a sample; dispersing by using a primary secondary amine (PSA) and octadecylsilane bonded-phase (C18) matrix to purify an extracting liquid; then, carrying out GC-NCI-MS detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the GC-NCI-MS detecting method, the average recovery rate is 86.3-94.3%, the average relative standard deviation (RSD) is 4.6-8.6%, and the detection limit is lower than 1.12mu g/kg; and the GC-NCI-MS detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the GC-NCI-MS detecting method, the technical requirements of Korea, Japan, European union and other countries on security detection of corresponding products can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of GC-NCI-MS method for measuring the residues of fenpyrafen in fruits and vegetables, more specifically, adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure The invention discloses a method for the residual content of pyrazafen, which belongs to the technical field of determination of pesticide residues. Background technique [0002] Cyenopyrafen (Cyenopyrafen) is a new type of pyrazole acaricide developed by Nissan Chemical Company in 2009. It is mainly used to control harmful mites such as red spider mites on fruit trees, vegetables and green peppers. The chemical name is (E)-2- (4-tert-butylphenyl)-2-cyano-1-(1,3,4-trimethylpyrazol-5-yl)enyl 2,2-dimethylpropionate, English Chemistry The name is (E)-2-(4-tert-butylphenyl)-2-cyano-1-(1,3,4-trimethylPyrazol-5-yl)vinyl 2,2-imethylpropionate, and the CAS accession number is 560121-52- 0,...

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. Pyrenifen is an electronegative compound, but so far there has been no report on the residues of Pyclofenac in vegetables and fruits. The report of GC-NCI-MS detection method, therefore, it is of great significance to establish the detection method of gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively analyze the residues of fenpyrafen in vegetables and fruits

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