Accelerated solvent extraction (ASE) is one of the most recent solid-phase extraction methods and has caught on all over the world in numerous laboratories. Until now it was not known that this device is also very suitable for performing dialysis. In this study, development of a rapid dialysis procedure (RDP) was described that is based on the dialysis of persistent organic xenobiotics from triolein-containing semipermeable membrane devices (SPMDs) using ASE. All the operating parameters were optimized within the framework of usage. The RDP procedure was compared with the conventional dialytic recovery of target analytes under atmospheric pressure using spiked analytes and real field samples of SPMDs exposed to urban air. The main advantages of the RDP in comparison to the conventional dialysis are the speed, with up to 70 times faster taking only 40 min, and the considerable reduction in solvent consumption (by two-thirds) when SPMDs with standard configuration are used. Moreover, the RDP is also suitable as an analytical cleanup procedure for the same analytes from various types of lipid samples and other difficult matrixes using semipermeable membranes.