GC-EI-MS method for rapidly determining residual ametoctradin amount

Abstract

The invention discloses a GC-EI-MS rapid determination method for the residual amount of oxamethanil, which is mainly used for determining the residual amount of oxamethazone in animal-derived foods with high fat content. Use acetonitrile to homogeneously extract the residual oxaflustrobin in the sample. After the extraction solution is dispersed and purified by Enhanced Matrix Removal (EMR) matrix, extracted and concentrated by stripping tube, gas chromatography-electron bombardment ion source- For mass spectrometry (GC-EI-MS) detection, a blank matrix solution without the pesticide to be tested was used to establish a calibration standard working curve, and the external standard method was used for quantification. The average recovery rate of this method is 90.2%-92.6%, the average relative standard deviation (RSD) is 5.8%-8.6%, and the detection limit is lower than 6.69 μg / kg. Strong characteristics, good repeatability, and accurate qualitative and quantitative advantages. It can meet the technical requirements of the United States, the European Union, Japan and other countries for corresponding product safety testing, and provide strong technical support for ensuring the food safety of our people and the healthy development of foreign export trade.

Description

Technical field [0001] The present invention relates to a GC-EI-MS rapid determination method for flufenoxazone residues, more specifically it uses gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively determine pork and beef , Mutton, chicken and other animal muscles and products and other high-fat animal-derived foods, methods for the content of pyraclostrobin residues belong to the technical field of pesticide residue determination. Background technique [0002] Ametoctradin is a new fungicide developed by BASF. Its trade name is Initium and its chemical name is: 5-ethyl-6-octyl[1,2,4]triazolo[1,5- a] Pyrimidine-7-amine, chemical formula is C15H25N5, structural formula is: [0003] [0004] Ametoctradin belongs to the s-triazolopyrimidine compound. It acts as an inhibitor of mitochondrial respiration and can prevent fungal diseases of the class of oomycetes, such as downy mildew and various blights. Ametoctradin was...

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Problems solved by technology

[0006] At this stage, there are few studies on the determination of oxamethazone residues. The detection methods reported are mainly the detection methods of oxamethazone 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 oxamethazone residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. However, due to its high price, many detection methods Institutions, enterprises or scientific research institutes are not equipped with this instrument or have a small number of units. 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, mobile phases and It takes a long time to balance the system, which restricts the application of LC-MS / MS to a certain 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 method for the detection of oxaflustrobin 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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