A new method was developed for the efficient spectrophotometric determination of methylene blue (MB) dye in solutions. The method is based on a combined dispersive solid phase and cloud point extraction using Cu(OH)2 nanoflakes (as an adsorbent). Cu(OH)2 nanoflakes were synthesized by facile and fast methods and characterized using various techniques. The developed method is based on the adsorption of MB on the Cu(OH)2 nanoflakes and transfer into a surfactant-rich phase using Triton X-114 as a nonionic surfactant. Subsequently, MB dye is desorbed from Cu(OH)2 nanoflakes using a mixture of nitric acid and methanol solution and determined by UV-Vis spectrophotometry. The effects of pH, amount of Cu(OH)2 nanoflakes, volume (concentration of Triton X-114), and temperature were investigated by designing experiments using response surface methodology (RSM). A quadratic model was utilized to predict the variables. Analysis of variance (ANOVA) was applied for the analysis of variables and their interactions, and optimal conditions were established. The results demonstrated logical agreement between experimental and predicted values of the response owing to high F value, low P value, and low lack-of-fit. The calibration graph was linear in the range of 2.0-350.0 μg L-1 of MB dye with a correlation coefficient (R) of 0.9996. The limits of detection and quantification were found to be 0.65 and 2.05 μg L-1, respectively. The developed method was successfully applied to different water samples, thereby confirming the applicability of the approach. Graphical Abstract Proposed procedure.