In this work, a sensitive tandem cloud-point extraction (CPE) method with a solvation system was employed to detect aspirin in various pharmaceuticals. Aspirin, in a dilute acidic solution, formed a complex with Zn(II) ions ([Zn(II)-aspirin] complex), which was then extracted using two different surfactant systems - nonionic surfactant Triton X-100 and a mixture of surfactants (SDS-Tween 80). The extracted complex was subsequently determined using spectrophotometry at a wavelength of 293 nm for Triton X-100 and 231 nm for SDS-Tween 80. The parameters for extraction, including HCl and Zn(II) concentration, temperature, heating time, and solvent used to dissolve the cloud point layer, were thoroughly investigated. Highperformance liquid chromatography (HPLC) was used as the standard method to compare the quantitative analysis of the cloud-point extraction-onium system.