An improved, simple gas chromatography-flame ionization detection (GC-FID) method was developed for measuring the products of acetone-butanol-ethanol (ABE) fermentation and the combined fermentation/separation processes. The analysis time per sample was reduced to less than 10 min compared to those of a conventional GC-FID (more than 20 min). The behavior of the compounds in temperature-programmed gas chromatographic runs was predicted using thermodynamic parameters derived from isothermal runs. The optimum temperature programming condition was achieved when the resolution for each peak met the analytical requirement and the analysis time was shortest. With the exception of acetic acid, the detection limits of the presented method for various products were below 10 mg/L. The repeatability and intermediate precision of the method were less than 10% (relative standard deviation). Validation and quantification results demonstrated that this method is a sensitive, reliable and fast alternative for conventional investigation of the adsorption-coupled ABE fermentation process.