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A biomass-derived sponge-like carbonaceous aerogel was prepared through a two-step procedure, including hydrothermal carbonization and freeze-drying process. The aerogel was employed as the solvent holder for liquid-phase microextraction of organophosphorus pesticides, ethion, and chlorpyrifos (as the model compounds), prior to determination by secondary electrospray ionization-ion mobility spectrometry. The carbonaceous aerogel is an appropriate candidate to be used as the solvent holder due to some properties such as three-dimensional structure, porous nature, and very low density. So, the aerogel, including extraction solvent, can tumble on the top of the sample solution, without loss of solvent during its agitation. A comparison of the extraction efficiency was performed at similar conditions between the proposed method and single-drop microextraction, as well as hollow-fiber solvent bar microextraction. Different parameters affecting the extraction efficiency, such as stirring rate, salt concentration, temperature, and extraction time were investigated by using the response surface methodology. The linear dynamic range was in the ranges 1–30 and 1–70 μg L−1 with regression coefficients of 0.9973 and 0.9956 for ethion and chlorpyrifos, respectively. The limit of detection was 0.09 and 0.21 μg L−1 for ethion and chlorpyrifos, respectively. The method was used for extracting analytes from environmental water and vegetable samples, with the spiking recoveries in the range 80–121%. [ABSTRACT FROM AUTHOR]

Thin film nanofibers containing ZnTiO3 nanoparticles were used for rapid and efficient evaporation of solvents as used to extract analytes by dispersive liquid-liquid microextraction (DLLME). The method is referred to as thin film evaporation (TFE). A combination of DLLME and TFE was applied to the extraction and preconcentration of the pesticide chlorpyrifos (as a model compound) prior to analysis by ion mobility spectrometry. The ZnTiO3 nanoparticles were placed on polyacrylonitrile nanofibers which increases the porosity and surface area in the TFE process, thus causing fast and complete evaporation of solvents. The effects of sample pH value, extraction solvent and its volume, disperser solvent and volume, centrifugation time, evaporation time, and desorption temperature were optimized. The relative standard deviations of intra- and inter-day analyses were found to be 3% and 7%, respectively. The method has a linear dynamic range that covers the 0.10-3.0 μg.L−1 chlorpyrifos concentration range, the limit of detection is 0.04 μg.L−1, and the enrichment factor is up to 5400 in case of spiked samples. Some spiked field samples were analyzed and the relative recoveries ranged between 99 and 111%. When applied along with ion mobility spectrometry, the interferences caused by solvent are found to be reduced in the ionization source. This makes it possible to select a variety of solvents as needed for sample extraction.Schematic presentation of dispersive liquid-liquid microextraction (DLLME) combined with thin film evaporation (TFE) for rapid vaporization of extraction solvent: Application to the pre-concentration of chlorpyrifos prior to its quantification by corona discharge-ion mobility spectrometry (CD-IMS). [ABSTRACT FROM AUTHOR]