A kind of gc-nci-ms determination method of fipronil residues

Abstract

The invention discloses a GC-NCI-MS method for measuring residual quantity of flubendiamide. The method is mainly used for measuring the content of residual flubendiamide in complex matrix food agricultural products such as cereal grains and animal derived foods. The method comprises the following steps: homogenizing and extracting the residual flubendiamide in the sample by using acetonitrile or an acetonitrile solution containing 1 percent of acetic acid, purifying and concentrating by using a C18 / PSA solid phase extraction column, performing gas chromatography-negative chemical ion source-mass spectrum (GC-NCI-MS) detection, establishing a corrected standard curve by adopting a blank matrix solution without to-be-detected pesticides, and quantifying by virtue of an external standard method. According to the method, the average recovery rate is 84.2-93.2 percent, the average relative standard deviation (RSD) is 4.6-6.9 percent, the detection limit is lower than 1.44mu g / kg, and the method has the advantages of simplicity and convenience in operation, rapidness, good impurity removal effect, high sensitivity, strong characteristic property, high repeatability and qualitative and quantitative accuracy. The residual limit of 0.01mg / kg in the corresponding food safety inspection in America, Japan, European Union and other countries can be met, namely the technical requirement on uniform limit is met, and a powerful technical support is provided for guaranteeing the food safety and sound export abroad trade development of people in China.

Description

technical field [0001] The present invention relates to a kind of GC-NCI-MS measuring method of flubendiamide residue, more specifically adopt 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 residual flubendiamide 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] Flubendiamide (Flubendiamide), trade name Longge, is a new type of phthalamide insecticide developed by Japanese pesticide company (known as Co., Ltd.), which has good activity against almost all lepidopteran pests , not only has excellent activity on both adults and larvae, but also has a fast acting speed and a long lasting effect. The effect on rice stem borer and leaf roller is absolutely top-notch. The...

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Problems solved by technology

Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometers (GC-MS), and are generally equipped with negative chemical ion sources (NCI). Now many types of pesticides contain electronegative groups, organochlorines and pseudo Pyrethrin pesticide molecules mostly contain strong electronegative groups such as -F, -Cl, -Br or -COO-; organophosphorus pesticide molecules mostly 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. Flubendiamide is an electronegative compound. 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 effect 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 flubendiamide residues in grains and animal-derived foods

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