GC-EI-MS (gas chromatography-electron impact ionization-mass spectrometry) measuring method of residual quantity of spirotetramat in fruit and vegetable

Abstract

The invention discloses a GC-EI-MS measuring method of the residual quantity of spirotetramat in fruit and vegetable. The method comprises performing homogeneous extraction on spirotetramat residue in a sample through acetonitrile or an acetonitrile solution containing 1% of acetic acid; performing dispersed purification on extracted solution through ethylenediamine-N-propyl silicane (PSA) and octadecyl silane bonded phase (C18) matrix; then performing GC-EI-MS detection, establishing a calibration standard curve through blank matrix solution not containing pesticide to be measured, and performing quantitation through the external standard method. The GC-EI-MS measuring method of the residual quantity of spirotetramat in fruit and vegetable achieves an average recovery rate of 86.4-93.2%, an average relative standard deviation (RSD) of 4.1-7.4% and a detection limit lower than 2.87 mu g / kg, has the advantages of being convenient and rapid to operate, high in sensitivity and repeatability and accurate in quantitation and quantification, can meet the technical requirements of the corresponding product safety inspection of nations such as the U.S., Japan, the European Union and Canada, and provides powerful technical support for food safety of people and healthy development of export trade in China.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS determination method of spirotetramat residual amount in fruits and vegetables, more specifically adopts gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively measure vegetables and fruits The method for the content of spirotetramat remaining in pesticides 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 resistant to existing insecticides, and at the same time, it can be used as an important sp...

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Problems solved by technology

[0006] At this stage, there are few studies on the determination of spirotetramat residues in vegetables and fruits, and the reported detection methods all use liquid chromatography-tandem mass spectrometry (LC-MS / MS) to determine the residues of spirotetramat in vegetables and fruits 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 have a small number of equipment. , 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, which restricts to a certain extent Applications 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 spirotetramat residues in vegetables and fruits, therefore, establish gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) qualitative and quantitative analysis of spirotetramat in vegetables and fruits The detection method of tetratetramat residue is of great significance

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