A large variety of pesticides have been used in the agriculturearea to raise the quality, extend and yield storage life of crops.However, the use of pesticides has been greater than before now a day dueto the growing rapid urbanization and population. The nonstop uses ofthese pesticides have resulted in pollution of the environment and alsocaused risk to human health. For the rapid detection of selective phenthoate pesticides, we developed a simple and highly sensitive spectrophotometric method based on azo-coupling reaction. After a simple pretreatment of phenthoatewith a diazotized solution,the resulting is rapidly undergoing azo-coupling reaction with 4-aminoazobenzene with adramatic color change only in few minutes.Finally, we successfully applied the concentration of phenthoate pesticides on vegetable, fruit, water, and soil samples. In this method, we found the absorption maxima of the orange dye compound was measuredat480nm.ThecolorsystemobeysBeer’slawinthefollowingworkingrangeof5µg to 40 µg in a final solution of 25 mL. The molar absorptivity, Sandell’s sensitivity, standard deviation, and the relative standard deviation was found to be 1.083X107L mol-1 cm-1, 0.99X10-5µg cm-2, ±0.003 and 0.89% respectively. This method is simple, sensitive, andfree from interferences of other pesticides and diverse ions. Other pesticides do not interfere with the proposed method. The method is highly reproducible and has been successfully applied for the determination of phenthoate insecticides in vegetables and fruit samples.