An extraction method using mixed catanionic surfactants of trimethyltetradecyl ammonium bromide (TTAB) and sodium dodecyl sulfate (SDS) was developed for preconcentration of organophosphorus pesticides (OPPs) before analysis by high performance liquid chromatography (HPLC). The studied OPPs are azinphos-methyl, parathion-methyl, fenitrothion, diazinon, chlorpyrifos, and prothiophos. The optimum extraction condition was 10 mmol L⁻¹ SDS and 0.5 mmol L⁻¹ TTAB in the presence of 10% (w/v) NaCl and equilibration at room temperature. The concentrated target pesticides were subsequently analyzed using a Symmetry C8 column, gradient elution of acetonitrile and water, at a flow rate of 0.8 mL min⁻¹, and detection at 210 nm. Enrichment factors were found in the range of 16–30. The limits of detection of the studied OPPs were 0.001–0.01 mg L⁻¹ which are below the maximum residue limits (MRLs) established by the European Union. Good repeatability (n = 5) and reproducibility (n = 15) were obtained with the relative standard deviation (RSD) below 2% for retention time and below 9% for peak area, respectively. The validation of the proposed method for fruit sample analyses was carried out by matrix matched calibration. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used for sample preparation before extraction and preconcentration. Recovery of the fortified samples at three levels (0.25, 1.50 and 2.50 mg kg⁻¹) was higher than 80.9% (on average) for all studied fruit samples (pomelo and pineapple). No detectable residues of OPPs in samples were found.