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Based On UPLC-MS/MS Analysis Of Veterinary Drug And Pesticides Residues

Posted on:2011-02-06Degree:MasterType:Thesis
Country:ChinaCandidate:K P ChengFull Text:PDF
GTID:2121360305974833Subject:Agricultural Products Processing and Storage
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Because of slather using pesticides and veterinary drugs, it promoted the rapid development of agriculture; meanwhile, it also endangered the quality and safety of food. In recent years China has broken out many food safety incidents, so, foreign countries have a confidence crisis about the food quality and safety of our country. Especially since the global financial crisis broken out in 2008, lots of countries and regions in the world have make more stringent trade protection measures, and some developed countries have continued to strengthen its technology, and set the high threshold residue limits for harmful substances in import-food, which result in China's food exports trouble. by contrast with the Europe-US and other developed countries.This paper researched the method for determination of pesticides and veterinary drug residues in food based on UPLC-MS/MS technology. The relevant work I made is as follows: (1) Study on establishing the UPLC-MS/MS methods and its quality control, (2)Research on the purification, extraction and determination of nanafroin residue in 13 different kind of food of animal food origin based on UPLC-MS/MS technology, (3)Study on based he purification, extraction and determination of simazine, carboxin, difluron and rotenone residues in tea based on UPLC-MS/MS method.The results obtained by experimentwere as follow:1. Established an extraction method to extract nanafrocin residue in 13 different kind of food of animal food origin. It was extracted with ethyl acetate and acetonitrile, using n-hexane to discard the fat, calibrate the volume to scale by Tris base solution, the method can effective extract the target material. The mean overall recoveries of nanafrocin varied from 71% to 101%, RSD was 2.8 %-11.83 %2. Established a fast, simple and UPLC-MS/MS to analysis nanafrocin residue in 13 different kind of food of animal food origin. The researchers applied a C18 stationary phase coupled to triple quadrupole tandem mass spectrometry in negative electrospray mode. The limit of detection (LOD) was 0.005 mg/kg and the limit of quantification (LOQ) was 0.01 mg/kg in the matrixes. The detector responses were found to be linear over the range 0.01-0.1 mg/kg in each matrix. In conclusion, identification and quantification of nanafrocin residues in foodstuffs of animal origin were successfully achieved using LC-MS/MS. The method can be used to analyze the nanafrocin efficiently. 3. A method for simultaneous determination of simazine, carboxin, diflubenzuron and rotenone in green tea was developed. Ethyl acetate was used to extract the residues after green tea sample was infiltrated in saturated aqueous sodium chloride solution, and the sample was cleaned up with PSA, C18 and graphitized carbon black powder. After that, the ethyl acetate supernatant was concentrated by the nitrogen evaporator. The residues were dissolved with mobile phase and syringe filtered using a 0.22μm nylon filter, tested by UPLC-MS/MS. The average recoveries of 77.4%-95.3%, and the RSD is 4.2%-11.8%.4. Chromatographic separation was performed on an ACQUITY UPLC? HSS T3 column (2.1 mm×100 mm, 1.8μm) using gradient elution. The positive ionization mode was used and the ions were monitored in the multiple reaction monitoring (MRM) mode. The limit of detection (LOD) is 0.005 mg/L and the limit of quantitation (LOQ) is 0.001 mg/L all of the three substances.The study on pesticide and veterinary drug residue limits and testing criteria in China the lagged somewhat. In order to safeguard the international impress of Chinese food, to adapt to fierce competition in international trade, and to meet the needs of food safety, we need to establish simple, practical and method to analysis the pesticides and veterinary drug residues in food.
Keywords/Search Tags:veterinary drug, pesticides, residues analysis, UPLC-MS/MS, QuEChERS
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