GC-NCI-MS determination method for cyenopyrafen residual quantity

Abstract

The invention discloses a GC-NCI-MS determination method for the cyenopyrafen residual quantity. The method is mainly used for determining the content of cyenopyrafen residues in complex matrix food-grade agricultural products such as grains and animal-origin foods. Acetonitrile or acetonitrile solution containing 1% of acetonitrile is used for extracting the cyenopyrafen residues in a sample in a homogeneous mode, a C18/PSA solid-phase extraction column performs purification and concentration, GC-NCI-MS detection is performed, a corrected standard curve is established by the adoption of blank matrix solution not containing pesticides to be determined, and an external standard method is adopted for quantification. According to the method, the average recovery rate is 85.8-91.4%, the average RSD is 4.0-7.0%, the detection limit is lower than 0.44 microgram/kg, and the method has the advantages of being easy and convenient to implement, rapid, good in impurity removal effect, high in sensitivity and characteristic feature, good in repeatability and accurate in quality determination and quantification. The method can meet the requirement of the residue limited quantity of 0.01 mg/kg for corresponding food safety inspection in Japan, EU, Korea and other nations and namely the technical requirement of the uniform standard and will provide forceful technical supports for guaranteeing food safety of Chinese and health development of export trades.

Description

technical field [0001] The present invention relates to a kind of GC-NCI-MS determination method of the residual amount of pyraclofen, more specifically, it adopts gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-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-bu...

AI Technical Summary

Problems solved by technology

Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometer (GC-MS), and are generally equipped with negative chemical ion source (NCI). Now many types of pesticides contain electronegative groups, organochlorine and pseudo Most pyrethroid pesticide molecules contain strong electronegative groups such as -F, -Cl, -Br or -COO-; most organophosphorus pesticide molecules contain =S, -OR, -P, -O-, -Cl, or -P=O and other electronegative groups; and most of the new pesticides developed in recent years contain -F groups. Therefore, the use of GC-NCI-MS can facilitate the multi-residue analysis of various pesticides. Compared with MS, it can obtain better anti-interference ability, lower sensitivity and better selectivity. Pyridofen is an electronegative compound, but so far there has been no report on the residues of Pyclofenac in vegetables and fruits. In the report of GC-NCI-MS detection method, due to the complex matrix of food and agricultural products such as grains and animal-derived foods, it is necessary to establish a sample pretreatment method and instrument analysis conditions with good purification effects to meet the detection requirements. Therefore, the establishment of gas chromatography- Negative Chemical Ion Source-Mass Spectrometry (GC-NCI-MS) is of great significance for the qualitative and quantitative analysis of cyfenpyrid residues in grains and animal-derived foods

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