Development of a method based on dispersive liquid–liquid microextraction followed by partial vaporization of the extract for ultra–preconcentration of some pesticide residues in fruit juices

A new simple and efficient method has been developed for the ultra-preconcentration of multiclass pesticide residues including penconazole, chlorpyrifos, ametryn, clodinafop-propargyl, diniconazole, oxadiazon, and fenpropathrin from some fruit juice samples based on evaporation of the sedimented organic phase obtained from dispersive liquid-liquid microextraction. The enriched target analytes were analyzed by gas chromatography-flame ionization detection. In the microextraction procedure, a mixture of iso-propanol as a disperser and 1,2-dibromoethane as an extraction solvent is quickly injected into an aqueous phase containing the analytes and centrifuged. Afterward, the sedimented phase is transferred into a special shaped vaporization vessel and vaporized with nitrogen gas stream until remaining about 2 µL of it. Eventually, 1 µL of the remained sedimented phase is removed and analyzed by separation system. The optimum extraction and disperser solvents were found to be 1,2-dibromoethane and iso-propanol, respectively. In addition, the optimum pH range was 6-8, and nitrogen gas stream at a flow rate of 90 mL min-1 in a downward oriented vessel was applied. Eventually, the limits of detection and quantification were obtained in the ranges of 45-78 and 149-261 ng L-1, respectively. Relative standard deviations at the concentrations of 300, 500 and 1000 ng L-1 of each analyte were ranged between 2.2% and 5.8% for intra-day (n = 6) precision. Inter-day (n = 3) precision at a concentration of 500 ng L-1 of each analyte was obtained in the range of 4.9-7.1%. In addition, enrichment factors and extraction recoveries were ranged from 1382-2246 and 55-89%, respectively. Finally, the method was successfully utilized in analysis of the target pesticides in the selected juices.