A sensitive method for extraction and determi- nation of three organophosphorus pesticides (chlorpyri- fos, diazinon, phosalone) using a supramolecular solvent (SUPRAS) made of inverted hexagonal aggregates of alkanol and high-performance liquid chromatography with ultraviolet detection (HPLC–UV) was developed. The stud- ied factors were alkanol amount, THF percentage (v/v), pH and vortex time. According to the full factorial design results, the effective parameters were alkanol amount, THF percentage (v/v) and pH. Then, a CCF was applied to obtain optimal conditions. The optimized conditions were obtained at 100 mg of alkanol, 5% of THF and pH 3.9. The limits of detection of pesticides were 0.5–1.3 ng/mL. The linearity was 1.6–500.0 ng/mL for different pesticides. Relative standard deviations for intra- and inter-day extrac- tion of pesticides were 3.3–5.0 and 5.1–6.3, respectively, for ive measurements. The method was also successfully applied for the determination of the pesticides in fruit juice and tap water samples.