GC (Gas Chromatograph)-EI (Electronic Impact Ionization)-MS (Mass Spectrometry) determining method of residual quantity of fluxapyroxad

Abstract

The invention discloses a GC (Gas Chromatograph)-EI (Electronic Impact Ionization)-MS (Mass Spectrometry) determining method of the residual quantity of fluxapyroxad. The GC-EI-MS determining method is mainly used for determining the content of residual fluxapyroxad in complex-matrix food and agricultural products of cereal grains, animal derived food and the like. The GC-EI-MS determining method comprises the following steps: homogeneously extracting the residual fluxapyroxad in a sample by using acetonitrile or an acetonitrile solution containing 1 percent of acetic acid; carrying out GC-EI-MS detection after purifying and concentrating by using a C18/PSA (Primary Secondary Amine) solid-phase extraction column; building a corrected standard work curve by adopting a blank-matrix solution which does not contain to-be-detected pesticide; quantifying through an external standard method. According to the GC-EI-MS determining method of the residual quantity of the fluxapyroxad, disclosed by the invention, the average recovery rate is 84.6 to 103.1 percent, the average RSD (Relative Standard Deviation) is 3.2 to 8.4 percent, and the detection limit is lower than 1.01 mug/kg; the GC-EI-MS determining method has the advantages that the operation is convenient and fast, the impurity removing effect is good, the sensitivity is high, the characteristic performance is strong, the repeatability is good, and qualitativeness and quantitativeness are precise; the technical requirements on safety detection of corresponding products of countries of America, EU (European Union), Japan and the like can be met, and a powerful technical support is provided for ensuring the safety of food for people in China and the healthy development of export trade.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS determination method of flufenapyroxamide residual amount, more specifically adopts gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively measure grain, pork, The invention relates to a method for residual flufenapyroxamide content in animal and plant-derived foods with complex matrices such as beef, mutton, chicken and other animal muscles and products, and belongs to the technical field of determination of pesticide residues. Background technique [0002] Fluxapyroxad is a succinate dehydrogenase inhibitor fungicide developed by BASF. Chemical name: 3-difluoromethyl-1-methyl-N-(3',4',5'-trifluorobiphenyl-2-yl)-1H-pyrazole-4-carboxamide; molecular formula: C18H12F5N3O ; Relative molecular mass: 381.3; Melting point: 157°C; Relative density: 1.42. Solubility in solvents (g / L, 20°C): acetone > 250, acetonitrile 168, ethyl acetate 123, m...

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Problems solved by technology

[0006] At this stage, there are few studies on the determination of flufenapyroxamide residues. The reported detection methods are mainly the detection methods of flufenapyroxamide 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 flufenapyramide 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 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 fluxapyroxad residues in food and agricultural products. Fluxapyroxamide is an electronegative compound. Since the matrix of food and agricultural products such as grains and animal-derived foods is relatively complex, the purification effect must be established Good sample pretreatment methods and instrumental analysis conditions can meet the detection requirements. Therefore, the establishment of gas chromatography-electron impact ion source-mass spectrometry (GC-EI-MS) qualitative and quantitative analysis of flufenapyramide in grains and animal-derived foods The detection method of residue is of great significance

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