A method for measuring VPGs using Orbitrap mass spectrometry was developed and used to identify the VPGs most indicative of smoke exposure in grapes and wine in CA. Guaiacol, 4-methylguaiacol, cresol and phenol rutinosides, syringol and 4-methylsyringol gentiobiosides, cresol pentose glucoside, and phenol glucoside were consistently found at elevated concentrations (>20 µg/L) in smoke-affected wine. These concentrations were several-fold higher than those of wines from vintages minimally affected by smoke. Satellite imaging data were used to compare the location and density of smoke plumes during the 2018 and 2020 wildfire seasons. Measurement of the above subset of VPGs in grapes sampled during 2018 and 2020 showed they were positively correlated with total glycoconjugates (i.e., the sum of cresol rutinoside, guaiacol rutinoside, 4-methylguaiacol rutinoside, phenol rutinoside, syringol gentiobioside, and 4-methylsyringol gentiobioside concentrations), despite varied levels of total glycoconjugates.