A quick and reliable approach was reported to measure the perfume loss in a commercial soap sample after continued use. This work firstly studied the fragrance loss profile in soap scientifically combined and compared with traditional olfactory evaluation. Solid-phase microextraction (SPME), as a simple and effective adsorption and desorption technique, was selected here to eliminate the needs of organic solvents or complicated apparatus; more importantly, SPME kept the soap intact and made it available for continued study. Thanks to control of the sampling time and other extraction parameters, a consistent and reliable result was achieved, which was much better and more detailed than traditional olfactory evaluation done by human beings.