BACKGROUND Excessive or improper use of organophosphorus pesticides (OPPs) may adversely affect human health through the food chain. In the present study, a simple, rapid and effective analytical method was successfully established and used for the determination of OPPs quinalphos and its analogs in different food samples. RESULTS Under the optimized experimental conditions, five OPPs (quinalphos, triazophos, parathion, fenthion and chlorpyrifos‐methyl) exhibit a good linearity within a range of 0.02 to 2.0 μg mL−1. The detection limit range was 3.0 to 10.0 μg L−1 (signal‐to‐noise ratio = 3). The method was successfully used to detect and quantify the residues of quinalphos and its analogs in tomato, cabbage, barley and water samples; all spiked samples gave satisfactory recovery rates for the target analytes of between 82% and 98%, with a relative SD of 3.6% to 7.8%. CONCLUSION The results obtained show that the proposed method is an accurate, rapid and reliable sample pre‐treatment method with respect to giving a good enrichment factor and detection limit for determining quinalphos pesticide residues in different food samples. © 2019 Society of Chemical Industry