The saponification of silicone-polyester resins with tetramethyl ammonium hydroxide to liberate common polyols for subsequent derivatization and gas chromatographic analysis is described. Recoveries of common polyols from silicone-polyester resins and from cured and uncured paint films formulated with these polymers are compared. Qualitative analysis of several dibasic acids is also achieved. The sample size for the analysis is minimized.