In this study, the most effective salting-out effect has been examined in terms of application of various inorganic salts (NaCl, Na₂S0₄, NaHSO₃) using Alkali impregnated filter-Headspace-GC/FID. Five various VFAs (propionic acid (99.5%), r-butyric acid (99%), butyric acid (99%), i-valerie acid (99%), valerie acid (99%)) have been used. VFAs have been analyzed by adding 30%, 70%, 100%, 150%, 200% of different inorganic salts with HS-GC/FID. The efficiency of salting-out effect was obtained from the values of peak area in chromatogram. The most effective salting-out effect for applired inorganic salts was observed at 100% saturation. It was confirmed NaHSO₃ for salting-out effect was the best among inorganic salts. In addition, NaHSO₃ showed more efficiency of salting-out effect than NaCl as molecular weight of VFAs increases.