Study On Detection Methods Of Trace Urotopine In Food

The main content of this research is the determination methods of trace Urotropine infood. Mainly by the different food matrix as the research object, the methods of qualitativeanalysis and quantitative analysis were researched. The most suitable detection methods weregiven according to the requirements of testing institutions and law enforcement agencies. Themain research work and results are as follows:1、Study on analysis method of rapid screening of qualitativeThrough the study on the ultrasonic extraction method instead of the conventional directheating method, the pretreatment method for qualitative analysis of urotropine was improved.Experiments showed that, by using ultrasonic conditions of65℃,45KHz, extraction time10min, extraction rate of urotropine could effectively improve the decomposition productsand the sensitivity and accuracy. The qualitative analysis method was simple, easy to operate,suitable for field test and laboratory screening. However, in order to determine the specificcontent of urotropine, accurate quantitative analysis should be carried out.2、Study on Laser Raman method for rapid quantitativeMethod for the determination of urotropine in food by laser Raman spectroscopy wasestablished. The excitation wavelength is785nm, the excitation power is200MW, and thescanning time of20s, with(894cm-1+3cm^-1)Raman peaks as quantitative Raman peak.the linear regression equation of standard curve method for the determination wasY=6484.1X+28.685the correlation coefficient is R2=0.9999, and the relative standarddeviation was1.14%⁴.75%. The recovery rate was up to90.4%¹09.7%and the detectionlimit is0.05mg/kg. The sample pretreatment was simple. This method was rapid, accurateand sensitive, and has good reproducibility and short detection time. The interference of thesystem is small It was low cost, small and portable and the equipment operation is relativelysimple. The method was suitable for on-site rapid detection requirements.3、Study on the accurate and efficient UPLC-MS/MS methodUPLC-MS/MS method was established for the efficient and accurate determination ofurotropine in food. Purification of the samples were carried out by C18column, using C18SPE cartridge and multiple reaction monitoring under the mode of ESI+（MRM）model to detect. The object in Agilent ZORBAX Eclipse（50mm×2.1mm,1.7μ m）column wasseparated efficiently. About3min was taken to complete a analysis of a sample. Thecorrelation coefficient（R2, n=6）was greater than0.999and the test results were stable,sensitive. The linear range was1.0⁵0.0μ g/L of urotropine and the detection limit was0.5μg/kg（LOD, S/N=3）. the recoveries was86.8%¹02.7%and precision RSD was0.36%⁴.79%. The method was rapid, sensitive and suitable for the detection and confirmation ofurotropine in food products.