Quick GC (Gas Chromatograph)-MS (Mass Spectrometry)/MS determining method of residual quantity of fluxapyroxad

Abstract

The invention discloses a quick GC (Gas Chromatograph)-MS (Mass Spectrometry) / MS determining method of the residual quantity of fluxapyroxad. The GC-MS / MS determining method is mainly used for determining the content of residual fluxapyroxad in animal derived food which is high in fat content. The GC-MS / MS determining method comprises the following steps: homogeneously extracting the residual fluxapyroxad in a sample by using acetonitrile; carrying out GC-MS / MS detection after dispersing and purifying matrix of an extracting solution by using an EMR (Enhanced Matrix Removal) and extracting and concentrating by using a reverse extraction tube; 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-MS / MS determining method of the residual quantity of the fluxapyroxad, disclosed by the invention, the average recovery rate is 93.6 to 98.7 percent, the average RSD (Relative Standard Deviation) is 5.0 to 7.4 percent, and the detection limit is lower than 0.044 mug / kg; the GC-MS / 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-MS / MS rapid determination method of flufenapyramide residue, more specifically adopts gas chromatography tandem mass spectrometry (GC-MS / MS) to qualitatively and quantitatively measure pork, beef, mutton, chicken and other animals The invention relates to a method for residual flufenapyramide content in animal-derived foods with high fat content such as 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, methanol 53.4, toluene 20.0. The chemical struc...

AI Technical Summary

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

The use of gas chromatography-tandem mass spectrometry (GC-MS / MS) to analyze pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, high sensitivity, and strong selectivity. It can achieve multi-residue analysis of hundreds of pesticides, but so far no food and agricultural products There are reports on GC-MS / MS detection method of flufenapyroxamide residue in food, but so far there is no report on GC-MS / MS detection method of flufenapyroxad residue 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

Images