Application of hollow fiber-protected liquid-phase microextraction combined with GC-MS in determining Endrin,...

This paper introduces a novel and minimized sample preparation technique based on hollow fiber-protected liquid-phase microextraction that can be used in joint with gas chromatography-mass spectrometry (GC-MS) detection to extract three organochlorine pesticides-Endrin, Chlordane, and Dieldrin-from rice samples. To that end, a single-walled carbon nanotube (SWCNT) and a proper ionic liquid (IL) were ultrasonically dispersed and injected into the lumen of hollow fiber as the extraction phase for preconcentrating and extracting the target analytes from the rice samples. The effects of the type of nanoparticles, ILs, and desorption solvent on the efficiency of extracting the analytes were investigated based on the one-factor-at-a-time (OFAT) approach. In addition, other parameters influencing the extraction procedure were optimized using an experimental design that decreased the number of experiments, reagent consumption, and costs. Under optimized conditions, the limits of detection and quantification in determining mentioned pesticides varied between 0.019-0.029 and 0.064-0.098 ng mL^-1, respectively. The calibration graphs to measure Endrin, Chlordane, and Dieldrin were linear over the concentration range of 0.064-13.2, 0.098-16.7, and 0.092-11.4 ng mL^-1, respectively. The relative standard deviations for inter-day and intra-day analysis were below 7.06 and 4.75% for the triplicate determination of three organochlorine pesticides. Besides, the relative recoveries and standard deviations of Endrin, Chlordane, and Dieldrin for analyzing several Iranian rice samples were between 86.0-92.9% and 4.5-5.8%, respectively. The results were compared with other similar works in literature, proving that the proposed method is efficient and useful for routine monitoring of organochlorine compounds in food samples.