Short chain organic acids from acetic to caprylic play an important role in tobacco flavor, and may be present in the flavors added to the liquids used in electronic smoking devices (e-liquids). For this reason, the determination of the level of those acids is of interest. Until recently, the GC/MS analysis of these acids has been problematic due to the reactivity of the analytes within the column phase that lead to the lack of reproducibility of results. The use of a new GC column, DB-624UI from Agilent leads to much better reproducibility. In this study, the column has been used for the separation and GC/MS analysis of several short chain organic acids including acetic, propionic, iso-butyric, butyric, iso-valeric, valeric, 3-methylpentanoic, caproic, heptanoic and caprilyc in tobacco and e-liquids. The analysis in e-liquids can be done directly following the dilution of the sample in methanol and injection in the GC/MS instrument. However, the direct analysis of the acids in tobacco after extraction, for example with methanol or acetonitrile, shows significant interferences. For this reason, a solid phase extraction (SPE) step is necessary to clean up the extract. This is done with retention from an acetonitrile extract on a Strata SAX 500 mg/3mL SPE cartridge, and elution with methanol containing 5.0 mg/mL formic acid. The eluted samples generated very reproducible results. A set of 18 tobaccos and six different e-liquids were successfully analyzed for short chain organic acids by this procedure.