The tobacco (Nicotiana tabacum L.) cultivation and cigarettes manufacture industries discard huge amount of waste tobacco materials that have strong nicotine smell and contaminate the environment. A high-efficient procedure was developed for simultaneously extracting nicotine and solanesol from the waste tobacco leaf vein through the column-chromatographic extraction (CCE), followed by automatically separating and simply purifying them. Dried material powder was loaded into columns and eluted with the optimal extraction solvent of petroleum ether (PE):95% alkali ethanol (4:6). Greater than 96% extraction efficiency for both nicotine and solanesol was obtained with a 2-fold excess solvent of the material (v/w) through a cyclic CCE procedure in small-scale and scaled-up experiments. The extraction solution was separated into an ethanol-aqueous phase containing 98% nicotine and an ether phase containing 96% solanesol at pH 2.0. The ethanol-aqueous phase was vacuum-concentrated to aqueous, and 99% purity nicotine was obtained by ether fractionation of the aqueous at pH 10.0. Solanesol in the ether phase was purified to 93.1% by one time silica gel column chromatography. All processes were completed at room temperature and all solvents used were completely recovered for reuse. This work provides an extensively simplified procedure to economically utilize the tobacco wastes. (C) 2015 Elsevier B.V. All rights reserved.