GC-EI-MS rapid measurement method for penflufen residual amount

Abstract

The invention discloses a GC-EI-MS rapid measurement method for the penflufen residual amount.The method is mainly used for measuring the content of residual penflufen in animal derived food high in fat content.Residual penflufen in a sample is extracted with acetonitrile in a homogeneous mode, after dispersion and purification are conducted on an extracting solution through an enhanced matrix removal (EMR) product substrate and extraction through a back extraction pipe and concentration are conducted, gas chromatography-electron impact-mass spectrum (GC-EI-MS) detection is conducted, a corrected standard work curve is established through an empty substrate solution containing no to-be-measured pesticide, and external standard method quantitation is conducted.The average recovery rate of the method is 81.2-91.0%, the average relative standard deviation (RSD) is 4.8-7.8%, and the detection limit is lower than 3.81 micrograms per kilogram.The method has the advantages of being easy and convenient to operate, rapid, good in impurity removal effect, high in sensitivity, strong in characteristic feature, good in repeatability and accurate in qualifying and quantifying.The technical requirements of America, European Union, Japan and other countries for safety detection on corresponding products can be met, and powerful technical support is provided for ensuring food safety of people in China and healthy development of export trades.

Description

Technical field [0001] The present invention relates to a GC-EI-MS rapid determination method of fluconazole aniline residues, more specifically it adopts gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively determine pork, beef, The method for the content of trifluconazole residue in animal-derived foods with high fat content such as animal muscles and products such as mutton and chicken belongs to the technical field of determination of pesticide residues. Background technique [0002] Fluconazole aniline is a succinate dehydrogenase inhibitor fungicide developed by BASF. Generic name: penflufen; test code: BYF14182; chemical name: N-[2-(1,3-dimethylbutyl) Phenyl]-5-fluoro-1,3-dimethyl-1H-pyrazole-4-carboxamide; appearance: off-white powdery solid; melting point: 111°C; boiling point: decomposes before boiling point; decomposition temperature: 320°C; Vapor pressure: 1.2×10 -6 Pa (25°C); partition coefficient: Kowlo...

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Problems solved by technology

[0008] At present, there are few studies on the determination methods of flufenadine residues, and the detection methods reported are mainly the detection methods of flufenadine residues in vegetables and fruits. These detection methods are all based on liquid chromatography tandem mass spectrometry (LC-MS / MS) is a detection method for the determination of flufenapyridine residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of quickness, simplicity, and high sensitivity. However, due to its high price, many testing institutions and enterprises Or the scientific research institute has not configured this instrument or the number of equipment is small. 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. The time to balance the system restricts the application of LC-MS / MS to some extent

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 on the GC-EI-MS detection method of flufenapyridine residues in food and agricultural products

In addition, it is well known that the QuEChERS pretreatment technology has become the most widely used sample pretreatment method in the analysis of pesticide residues, but the QuEChERS method is mainly suitable for low-fat high-water substrates, such as most fruits and vegetables, in the face of high-fat content The capacity of the matrix is ​​limited, and it is generally necessary to add n-hexane degreasing, frozen sample extract degreasing and other steps, but the effect is limited

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