GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for residual quantity of cyantraniliprole 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 cyantraniliprole 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 cyantraniliprole 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 89.2-96.7%, the average relative standard deviation (RSD) is 3.5-8.8%, and the detection limit is lower than 0.53mu 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 America, Canada, European union, Japan 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 method of GC-NCI-MS determination cyantraniliprole residue in fruits and vegetables, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure residues in vegetables and fruits The method for the content of cyantraniliprole belongs to the technical field of determination of pesticide residues. Background technique [0002] Cyantraniliprole, also known as cyantraniliprole (cyantraniliprole), is a second-generation ryanodine receptor inhibitor insecticide successfully developed by DuPont after chlorantraniliprole. Formed from various polar groups on the benzene ring, compared with chlorantraniliprole, it has a wider spectrum of insecticidal activity, excellent control effect on piercing-sucking pests, and has better systemic properties , the market prospect is broad. The chemical name is 3-bromo-1-(3-chloro-2-pyridyl)-{4-cya...

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. Cytraniliprole 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 cyantraniliprole residues in vegetables and fruits

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