Methyl anthranilate (MA), ortho-aminoacetophenone (o-AAP), and furaneol contribute to the characteristic “native grape” and “cotton candy” aromas of Vitis labruscana grapes and their hybrids, e.g. ‘Concord’ and ‘Niagara’. Convenient measurement of these compounds is of interest to grape breeders who wish to either increase or decrease their concentrations in grape varieties. Previous approaches for measurement of these odorants either cannot measure all compounds in a single analysis, or else have detection limits above the sensory thresholds for the odorants (low µg/L). We evaluated the use of an optimized reverse phase solid phase extraction (SPE) approach prior to selected ion monitoring (SIM) GC-MS to achieve low µg/L detection limits for MA, o-AAP, and furaneol in a single analysis.