Aqueous solutions of sodium cumene sulfonate give quantitative and faster extraction of reserpine from Rauwolfia vomitoria as compared to the extraction using methanol. The extraction rate is influenced by intraparticle diffusion and increases with increasing temperature and hydrotrope concentration. The dynamic extraction data were fitted in a mass transfer model to evaluate diffusion coefficient of reserpine in the solid plant matrix. Amongst all hydrotropes, sodium cumene sulfonate, gave the best extraction and extraction rates of reserpine. The reserpine crystals recovered from aqueous hydrotrope solutions were much smaller in size and showed different morphology than those from methanol.