Accurate, robust, and wide-coverage analytical tools are needed in polyphenol research to deal with the high physicochemical complexity of the secondary plant metabolome. In this chapter, a novel method based on reversed-phase ultrahigh-performance liquid chromatography coupled with a diode array detector and mass spectrometry is presented, which enables high-throughput, comprehensive, and quantitative fingerprinting of a broad spectrum of phenolic compounds and related metabolites in different food products. The simplicity, low-cost, and excellent analytical performance of this method would facilitate its implementation in food science for quality control and authenticity purposes.