The co-precipitation of loperamide hydrochloride (LPM) and polyethylene glycol (PEG) using aerosol solvent extraction system (ASES) was examined. Scanning electron microscopy - energy dispersive X-ray spectroscopy (SEM-EDS) analysis showed that the co-precipitation was achieved in various LPM-PEG mass ratios with changes in its morphology. In 10-50% PEG mass ratios, angular-shaped particles were formed, whereas in 65-90% PEG mass ratios, irregular-shaped particles were formed. X-ray diffraction (XRD) analysis of the co-precipitates revealed that the LPM retained amorphous structure, while, on the other hand, the PEG retained crystalline structure. Fourier transform infrared (FT-IR) spectra indicated carbonyl function group of LPM and ether function group of PEG appeared in the co-precipitates. Results of a dissolution test showed that the co-precipitates of LPM-PEG had higher dissolution rate compared to that of the raw material and processed LPM with ASES. Taken together, the co-precipitation of LPMPEG was achieved using ASES and higher in its dissolution rate. EDS of 50% PEG precipitate showed that chlorine map (indicate LPM) and oxygen map (indicate PEG) are co-precipitate.