Previously published data show that high levels of fat (50%) affect the yield of volatile compounds during solvent-assisted flavour evaporation (SAFE). We present new data demonstrating that even low levels of fat (< 10%) lead to significantly lower yields of high boiling point volatiles during SAFE. Relative recovery during SAFE of a range of volatiles from a cheese extract was measured at varying fat concentrations (1.1–8.7%) using a single internal standard. Volatiles with higher boiling points had significantly lower relative recoveries, and volatiles were substantially less well recovered from higher fat extracts. When endeavoring to obtain solvent extracts of fatty foods for the purposes of GC-O, it is important to choose the extraction technique which produces solvent extracts closely representing the true composition of the food. We present dilution of solvent extracts prior to SAFE as a potential new approach for high-fat foods which enables high yields of volatiles regardless of boiling point. These data also show that in the absence of C13-labelled standards for quantitation, it is critical to maintain a consistent fat content between samples during SAFE.