Carbamates and organophosphorus (OPPs) pesticides are the most widely used pesticides. Therefore, it has been necessary to develop accurate analytical method for the identification and quantification of OPPs and carbamate pesticides in fruits and vegetables. Due to their physical chemical properties such as thermal instability and polarity, carbamates are difficult or even impossible to be analyzed using GC techniques without the time-consuming process of derivatization. Due to lower sensitivity of LC/UV, HPLC with fluorescence detection by post-column derivatization is the most widely used method for the analysis of carbamate pesticides in foods [1]. Most OPPs are easily analyzed by GC. Therefore, carbamates and OPPs are usually analyzed by liquid chromatography and gas chromatography, respectively. Just so, the procedure is time-consuming.