Determination of fenazaquin in water and tomato matrices by GC-MS after a combined QuEChERS and switchable solvent liquid phase microextraction.

This study presents the use of Quick Easy Cheap Efficient Rugged and Safe (QuEChERS) as an effective sample cleaning procedure and switchable solvent liquid phase microextraction (SS-LPME) as a preconcentration tool for the determination of fenazaquin by gas chromatography mass spectrometry (GC-MS) at ultratrace levels. After a thorough optimization process, 0.50 mL of switchable solvent, 1.5 mL of 1.0 M sodium hydroxide, and 15 s of vortexing were determined as optimum conditions of the SS-LPME method. The limit of detection (LOD) and limit of quantitation (LOQ) determined using the optimum method (SS-LPME/GC-MS) were 0.05 and 0.18 ng/mL, respectively. Compared with direct GC-MS determination of fenazaquin, the optimum method yielded about 800-fold enhancement in detection power of GC-MS. The method was applied to lake, irrigation canal, well, and wastewater samples. In order to test the method's applicability on fresh tomato samples, a QuEChERS method was used before applying the SS-LPME method. Matrix-matched calibration standards were used to enhance the accuracy of fenazaquin quantification in spiked tomato samples to obtain recovery results close to 100%.

Binary Dispersive Liquid-Liquid Microextraction Strategy for Accurate and Precise Determination of Micropollutants in Lake, Well and Wastewater Matrices.

In this study, a binary mixture in dispersive liquid-liquid microextraction was used for the preconcentration and determination of selected pesticides, pharmaceutical and hormone by GC-MS. A Box-Behnken experimental design was used to optimize the amounts of binary mixture, dispersive solvent and salt. The optimum parameters obtained were dichloromethane/1,2-dichloroethane binary mixture (200 µL), ethanol (2.0 mL) and potassium nitrate (1.0 g). Analytical performance of each analyte was determined under the optimum conditions and the lowest and highest detection limits calculated were 0.43 and 5.9 ng/mL. Low relative standard deviations were obtained even in the lowest concentrations in linear calibration plots, signifying high precision for the sample preparation procedure and instrumental measurement. Accuracy of the developed method and applicability to real samples was tested on well, lake, hospital and municipal wastewater. The percent recoveries acquired at different spiked concentrations were satisfactory (89%-108%), validating the accuracy of the method for the quantification of the analytes in the selected matrices.