Determination of organophosphorus pesticides using dispersive liquid–liquid microextraction combined with reversed electrode polarity stacking mode—micellar electrokinetic chromatography

A rapid and sensitive method using two preconcentration techniques, dispersive liquid–liquid microextraction (DLLME) followed by reversed electrode polarity stacking mode (REPSM) was developed for the analysis of five organophosphorus pesticides (OPPs) by micellar electrokinetic chromatography (MEKC). Parameters that affect the efficiency of the extraction in DLLME and preconcentration by REPSM, such as the kind and volume of the extraction and disperser solvents, salt addition, sample matrix and injection time were investigated and optimized. Under the optimum conditions, the enrichment factors were obtained in the range from 477 to 635. The linearity of the method for parathion, azinphos and fenitrithion was in the range of 20–1000 ng mL−1, and for malathion and diazinon in the range of 50–1000 ng mL−1, with correlation coefficients (r2) ranging from 0.9931 to 0.9992. The limits of detecton (LODs) at a signal-to-noice ratio of 3 ranged from 3 to 15 ng mL−1. The relative recoveries of five OPPs from water samples at spiking levels of 20 and 200 ng mL−1 for parathion, azinphos and fenitrithion, and 50 and 500 ng mL−1 for malathion and diazinon, were 69.5–103%. The proposed method provided high enrichment factors, good precision and accuracy with a short analysis time.