Solvent co-distillation was employed to isolate and collect the aroma compounds of tobacco, which were then determined by GC/MS. The major aroma compounds in the isolated mixture were quantified with the internal standard (methyl nicotinate) added. Compared with the simultaneous distillation extraction (SDE), the solvent co-distillation was fast, convenient, and easy to operate. The repeatability was satisfactory. The obtained result was comparable to those obtained from SDE.