GC-EI-MS method for rapidly determining residual aminobenzene pyrazolone amount

Abstract

The invention discloses a GC-EI-MS method for rapidly determining the residual aminobenzene pyrazolone amount.The method is mainly used for determining the residual aminobenzene pyrazolone amount in animal derived foods with high fat content.Acetonitrile is adopted to homogeneously extract the residual aminobenzene pyrazolone in a sample, the extracting solution is subjected to matrix dispersion and purification of an enhanced matrix removal (EMR) product and extraction by a reverse extraction tube and concentration are conducted, then gas chromatography-electron impact ionization-mass spectrometry (GC-EI-MS) detection is performed, a blank matrix solution containing no pesticide to be detected is adopted to establish a standard working curve for correction, and quantification is performed by adopting an external standard method.The average recovery rate of the method is 92.0%-93.4%, the average relative standard deviation (RSD) of the method is 4.6%-7.0%, the detection limit of the method reaches 2.19 micrograms / kilogram or below, and the method has the advantages of being simple and convenient to operate, rapid, good in impurity removal effect, high in sensitivity, good in characteristic performance and repeatability and accurate in qualititation and quantification, can meet the technical requirements for corresponding product safety detection of the United States, European Union, Japan and other countries and provides a powerful technical support for ensuring the people's food safety and healthy development of the abroad export trade of our country.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS rapid determination method of pyrazolone residual amount, more specifically adopt gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) qualitative and quantitative determination pork, beef The invention discloses a method for residual fenpyrazolone content in animal-derived foods with high fat content such as animal muscle and products such as mutton, chicken, etc., belonging to the technical field of determination of pesticide residues. Background technique [0002] Fenpyrazamine is a pyridine-based heterocyclic fungicide developed by Sumitomo Chemical Co., Ltd., which inhibits the pathogens of the ergosterol biosynthetic pathway, and shows effects on mycelial growth and spore germination and Inhibition of pollen tube growth. The CAS number is: 473798-59-3, the molecular formula is C 17 h 21 N 3 o 2 S, the molecular weight is 331.43, and the chemical structural formula...

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Problems solved by technology

[0006] At this stage, there are few studies on the determination methods of pyrazolone residues. The detection methods reported are mainly the detection methods of pyrazolone residues in vegetables and fruits. These detection methods are all using liquid chromatography tandem mass spectrometry (LC- MS / MS) is a detection method for the determination of pyrazolone 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 detection method of fenpyrazolone 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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