Study on the Sample Pretreatment Procedure and Determination by UPLC-MS in PhIP Chemical System

The sample preparation procedure and analytical method were developed for the determination of PhIP in chemical model system. The reaction system was freeze-dried by a lyophilizer,then extracted with alkaline ethyl acetate. Finally,the solvent was removed by nitrogen blower. The extract was separated on a BEH phenyl column,with 0.1% formic acid in acetonitrile-water as mobile phases in gradient elution. The qualitative and quantitative operation of PhIP is based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS). The results showed that linear range of PhIP was 0.5~15 ng/mL,the coefficient of determination was 0.999. The limits of detection and limits of quantitation for the PhIP was 0.110 and 0.332 ng/mL respectively. The average recoveries of all the compounds spiked in wine samples at three levels of 10,15,30 ng/mL were in the ranges of 78.16%,81.22%,82.03%,with the corresponding relative standard deviations (RSD) of 6.32%,5.40%,4.28%,respectively. The experimental results indicated that the method is simple,sensitive,accurate and can meet the requirement for the determination of PhIP in chemical model system.