Method for determining methamidophos in rice wine
A method of determination, a technology of methylamine, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that affect the quantitative accuracy of residue analysis and low recovery rate, and solve the problems of difficult to produce effective retention, high recovery rate, and advanced Effects that are easy to handle
Inactive Publication Date: 2011-08-17
中华人民共和国绍兴出入境检验检疫局
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Problems solved by technology
Because rice wine contains a lot of water and alcohol, and methamidophos is highly polar, the analysis method of methamidophos residues in other products will lead to low recovery rate, which will affect the accuracy of residue analysis and quantification
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Embodiment 1
[0073] A detailed description will be given below of specific embodiments of the present invention.
[0074] 1.1 Method summary
[0075] Methamidophos in yellow rice wine was extracted by Easy solid-phase extraction column and eluted with ethyl acetate, and then determined by gas chromatography-flame photometric detector (GC-FPD) for positive screening and quantification, using liquid chromatography-tandem Mass spectrometry (LC-MS-MS) was used for qualitative confirmation of positive samples.
[0076] 1.2 Reagent materials
[0077] 1.2.1 Acetone and ethyl acetate are pesticide residue grade reagents; water is ultrapure water (resistivity 18.2MΩ);
[0078] 1.2.2Easy solid phase extraction cartridge: 500mg / 3mL, Germany MN company;
[0079] 1.2.3T3 liquid chromatography column: length 100mm, inner diameter 2.1mm, filler particle size 3.0μm.
[0080] 1.2.4 Methamidophos standard stock solution: 100 μg / mL (Environmental Protection Research and Monitoring Institute of the Minist...
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Abstract
The invention discloses a method for determining methamidophos in rice wine and particularly discloses a method for detecting the content of methamidophos in rice wine by utilizing gas chromatography and liquid chromatography-tandem mass spectrometry. The method comprises the following steps: (1) extraction and purification: utilizing a solid phase extraction column to extract the methamidophos in the rice wine and using ethyl acetate to elute the methamidophos adsorbed on the solid phase extraction column; (2) preparation of matrix matched standard working solution; (3) qualitative screening and quantification by utilizing gas chromatography; (4) qualitative confirmation of positive samples by using liquid chromatography-tandem mass spectrometry; (5) blank test; and (6) result calculation and representation. The method has the following beneficial effects: the pretreatment operation is simple and practical, and the recovery rate of the methamidophos is high; and by adopting the matrix matched standard working solution, the problem of matrix effect of the methamidophos on the gas chromatograph is solved, and accurate quantification is implemented.
Description
technical field [0001] The invention relates to a qualitative and quantitative detection method for methamidophos pesticide residues in rice wine. Background technique [0002] Methamidophos is a high-efficiency organophosphorus pesticide with a wide range of insecticides, and is widely used in the cultivation of grains, vegetables and other crops. Due to its strong toxicity, it has been banned in some countries such as China and Japan. In January 2008, six ministries and commissions including the National Development and Reform Commission of the People's Republic of China issued the "Announcement on Stopping the Production of Five Kinds of Highly Toxic Pesticides including Methamidophos", prohibiting the use of five kinds of organophosphorus pesticides including methamidophos. [0003] In recent years, food safety emergencies have occurred frequently, and the requirements for the limit of pesticide residues in food have become more and more stringent at home and abroad. F...
Claims
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Inventor 胡贝贞董文洪宋伟华陶兴耀
Owner 中华人民共和国绍兴出入境检验检疫局