Abstract: Thin layer chromatography on acidic alumina without binder has been applied for the identification and separation of coumarone compounds. A series of coumarone compounds were chromatographed on acidic alumina, and factors such as adsorbent, solvent, particle size of alumina, and the extent of presaturation of the adsorbent, have been studied. The results showed that the technique of thin layer chromatography on acidic alumina (160 mesh) with petroleum ether:chloroform (1:1), petroleum ether:alcohol (1:1), or petroleum ether: dioxane (10:2) as developing agents, without presaturation of the adsorbent with the vapor of corresponding solvents, could be utilized satisfactorily for the purpose of identification and separation of coumarone compounds. The method was applied to the examination of furan-coumarine compounds in Peucedanum decursivum Maxim and Ligusticum jeholense Nak. et Kitaga. with satisfactory results.