Systematic research is still lacking on the content of hydrophilic compounds in Fu Brick Tea (FBT) from major Chinese production regions and their variation patterns during the processing of FBT. This study utilized optimized non-targeted (UHPLC-Q-Exactive Orbitrap-MS) and targeted (UHPLC-QqQ-MS) metabolomics to analyze 73 FBT samples from six regions of China and 30 samples from different stages of FBT processing. 573 and 74 hydrophilic compounds were respectively relatively and absolutely quantified for the first time. Among the 73 FBT samples, alkaloids were the most abundant (26221.76-36701.75 mg/kg), followed by soluble sugars (211372.59-26112.85 mg/kg), organic acids (17014.07-23589.20 mg/kg), amino acids (6664.59-9791.46 mg/kg), nucleotides (1020.33-2175.16 mg/kg), and nucleoside (650.86-1446.26 mg/kg). During the processing of FBT, sugars, acids, nucleotides, and nucleosides increased, while amino acids decreased, and alkaloids slightly increased. This study enhances the understanding of hydrophilic compounds in FBT.