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

Abstract

The invention discloses a GC-EI-MS (Gas Chromatography-Electron Ionization-Mass Spectrum) detecting method for the residual quantity of cyenopyrafen in fruits and vegetables. The GC-EI-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-EI-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-EI-MS detecting method, the average recovery rate is 87.2-92.6%, the average relative standard deviation (RSD) is 4.0-6.5%, and the detection limit is lower than 1.33mu g/kg; and the GC-EI-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-EI-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-EI-MS method for measuring the residual amount of fenpyrafen in fruits and vegetables, more specifically, adopting gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively measure vegetables and fruits The invention discloses a method for the content of pyrazafen residues in pesticides, 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,...

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Problems solved by technology

[0006] So far, only one patent "a method for the determination of pyrazafen residues" has been retrieved, which establishes a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of pyrazafen residues in vegetables and fruits. Using LC-MS / MS to measure pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. However, due to its high price, many testing institutions, enterprises or research institutes have not equipped this instrument or have a large number of equipment. Since different compounds are detected by LC-MS / MS, different mobile phases or chromatographic columns need to be used, which requires constant replacement of chromatographic columns and mobile phases and takes a long time to balance the system, which restricts to a certain extent Application of LC-MS / MS

Gas chromatography-mass spectrometry (GC-EI-MS) equipped with electron bombardment ionization source has great advantages in analyzing pesticide residues in food and agricultural products. Since electron bombardment ionization source mass spectrometry is a universal detector, it can realize multi-residue analysis of hundreds of pesticides. It can be qualitative and quantitative at the same time, and the price is moderate. Therefore, various testing institutions and enterprises are equipped with gas chromatography-electron bombardment ion source-mass spectrometer (GC-EI-MS) to detect pesticide residues in food and agricultural products, but so far no See the report of the GC-EI-MS detection method of nitrile pyraclofen in vegetables and fruits, therefore, establish gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) qualitative and quantitative analysis of nitriles in vegetables and fruits The detection method of pyraclofen residue is of great significance

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