Comparative Study of Determination for Melamine in Dairy Products about Optimize Ultra Performance Liquid Chromatography Tandem Mass Spectrometry and High Performance Liquid Chromatography
The ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of melamine in dairy products was optimized and comparative experiments on high performance liquid chromatography(HPLC)was conducted.A double population t-test analysis on the experimental results of two detection methods was performed.The sample was extracted with 1%perchloric acid solution and acetonitrile and separated by high-speed centrifugation,then the supernatant was purified using a PCX solid-phase extraction column.Finally,melamine was eluted with 5%ammoniated methanol and concentrated in nitrogen for UPLC-MS/MS determination.The results showed that the correlation coefficient r2 of the quantitative curve equations for both HPLC and UPLC-MS/MS methods were greater than 0.995.At the addition levels of 1,2,and 10 times the limit of quantification,the recoveries were 87.8%～92.5%and 89.8%～94.2%with relative standard deviation(RSD)of 3.21%～5.24%and 5.05%～6.44%,respectively.There is no significant difference in the detection results between the two methods.The optimized UPLC-MS/MS method has a higher recovery rate and good reproducibility,which can be applied to practical daily sample determination.
UPLC-MS/MSHPLCdairy productmelaminedouble population t-test
万方数据
维普
