GC-EI-MS measurement method for cyenopyrafen residual amount

Abstract

The invention discloses a GC-EI-MS (gas chromatograph-electron ionization-mass spectrometry) measurement method for a cyenopyrafen residual amount. The method is mainly used for measuring the content of cyenopyrafen retained in complicated matrix food agricultural products such as grains and animal derived food. The method comprises the steps of extracting the cyenopyrafen retained in a sample by homogenizing acetonitrile or an acetonitrile solution with 1 percent of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-EI-ES detection, building a corrected standard curve for a blank matrix solution without pesticide to be detected, and carrying out quantification by an external standard method. According to the method, the average recycling rate is 81.9-89.0 percent, the average relative standard deviation (RSD) is 4.7-6.5 percent, and the detection limit is lower than 0.73 [mu]g / kg; the method has the advantages of simplicity and convenience in operation, quickness, good impurity removal effect, high sensitivity, high repetitiveness and accuracy in qualification and quantification. The technical requirement of 'uniform limit' on the 0.01 mg / kg residue limit of corresponding food safety detection of the countries such as Japan, European Union and Korea can be met.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS determination method of the residual amount of pyraclofen, more specifically, it 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 the content of pyrifenin residues 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] Cyenopyrafen (Cyenopyrafen) is a new type of pyrazole acaricide developed by Nissan Chemical Company in 2009. It is mainly used to control harmful mites such as red spider mites on fruit trees, vegetables and green peppers. The chemical name is (E)-2- (4-tert-butylphenyl)-2-cyano-1-(1,3,4-trimethylpyrazol-5-yl)enyl 2,2-dimethylpropionate, English Chemistry The name is (E)-2-(4-tert-b...

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Problems solved by technology

[0006] So far, only one patent "a method for the determination of pyrimidin residues" has been retrieved, which establishes a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of pyrimidin in vegetables, fruits and tea. The detection method of ester residues, the use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of fast, simple, and high sensitivity. However, due to its high price, many testing institutions, enterprises or research institutes have not equipped this instrument or configuration The number of units is small, because when 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 to balance the system. Restricts the application of LC-MS / MS

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 pyrazafen residues in food and agricultural products. Due to the complex matrix of food and agricultural products such as grains and animal-derived foods, a sample pretreatment method with good purification effect must be established to meet the detection requirements. Therefore, it is of great significance to establish a gas chromatography-mass spectrometry (GC-EI-MS) detection method for the qualitative and quantitative analysis of pyrazafen residues in grains and animal-derived foods

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