GC-EI-MS (Gas Chromatography-Electron Ionization-Mass Spectrum) detecting method for residual quantity of spirotetramat

Abstract

The invention discloses a GC-EI-MS (Gas Chromatography-Electron Ionization-Mass Spectrum) detecting method for the residual quantity of spirotetramat. The GC-EI-MS detecting method is mainly used for detecting the content of residual spirotetramat in complex-matrix foods and agricultural products such as cereal grains and animal-derived foods. The GC-EI-MS detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual spirotetramat in a sample; purifying and concentrating by using a C18 / PSA solid-phase extraction column; then, carrying out GC-EI-MS detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the GC-EI-MS detecting method, the average recovery rate is 81.4-89.3%, the average relative standard deviation (RSD) is 4.6-8.9%, and the detection limit is lower than 3.57mu g / kg; and the GC-EI-MS detecting method is simple and convenient to operate, rapid, good in impurity removal effect, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the GC-EI-MS detecting method, the technical requirements of America, European union, Japan and other countries on residual quantity limit in security detection of corresponding foods can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS assay method of spirotetramat residual amount, more specifically adopt 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 residual spirotetramat 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] Spirotetramat (Spirotetramat) is a new tetronic acid derivative insecticide developed and produced by Bayer Company of Germany. It has a wide insecticidal spectrum and a long duration of action. Mainly by interfering with the lipid biosynthesis of insects, it leads to larval death and reduces the reproductive ability of adults. Due to its unique mechanism of action, it can effectively control pests resi...

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Problems solved by technology

[0007] So far, there is no research report on the determination method of spirotetramat residues in grains and animal-derived foods. The detection methods of spirotetramat residues in fruits and vegetables are all using liquid chromatography (LC), liquid chromatography The determination of spirotetramat residues by tandem mass spectrometry (LC-MS / MS), 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

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 spirotetramat 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 qualitative and quantitative analysis of spirotetramat residues in grains and animal-derived foods

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