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A novel solid-phase microextraction (SPME) fiber coated with a sol-gel/nanoclay composite was prepared by the sol-gel technique involving the hydrolysis reaction of alkoxysilanes and the subsequent condensation reaction with hydroxyl groups of the nanoclay on a stainless steel wire. A method based on direct immersion SPME and gas chromatography-corona discharge ion mobility spectrometry was developed for the determination of four organophosphorus pesticides in aqueous samples. The effect of different experimental parameters on the extraction efficiency of the method was investigated. The sol-gel/nanoclay fiber showed higher extraction performance for the organophosphorus pesticides compared with Ppy/nanoclay, sol-gel coating, and three commercial fibers (polydimethylsiloxane (PDMS), PDMS/divinylbenzene (DVB), and polyacrylate (PA)). Limits of detection (LOD) and quantitation (LOQ) of the method were in the range of 0.003-0.012 and 0.01-0.02 μg L(-1), respectively. The calibration curves were linear in a concentration range from 0.01 to 2.0 μg L(-1) (r (2) > 0.995). The relative standard deviations for intra- and inter-day precision were 3.3-5.6 and 6.4-8.4 %, respectively. Fiber-to-fiber reproducibility for three prepared fibers was 7.4-10.2 %. Finally, the method was successfully applied for the extraction of the studied compounds from water samples. The relative recovery obtained for the spiked real-water samples were 86-104 %.

A novel method based on three-phase hollow fiber microextraction technique (HF-LPME) coupled with electrospray ionization-ion mobility spectrometry (ESI-IMS) was developed for the simultaneous determination of two antidepressant drugs (trimipramine and desipramine) in urine and plasma samples. The effects of various parameters such as type of organic solvent, composition of donor and acceptor phase, stirring rate, salt addition, extraction time, and temperature were investigated. Under the optimized conditions, the relative standard deviation was in the range of 5-6%, and the method quantitation limit (MQL) of utilizing HF-LPME/ESI-IMS was 5 μg/L for both drugs. The relative recoveries obtained by the proposed method from urine and plasma samples were in the range 94% to 97% for trimipramine and 92% to 96% for desipramine. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of trace amounts of trimipramine and desipramine in biological samples without any significant matrix effect.

A corona discharge ionization-ion mobility spectrometry (CD-IMS) with a novel sample inlet system was designed and constructed as a detector for capillary gas chromatography. In this design, a hollow needle was used instead of a solid needle which is commonly used for corona discharge creation, helping us to have direct axial interfacing for GC-IMS. The capillary column was passed through the needle, resulting in a reaction of effluents with reactant ions on the upstream side of the corona discharge ionization source. Using this sample introduction design, higher ionization efficiency was achieved relative to the entrance direction through the side of the drift tube. In addition, the volume of the ionization region was reduced to minimize the resistance time of compounds in the ionization source, increasing chromatographic resolution of the instrument. The effects of various parameters such as drift gas flow, makeup gas flow, and column tip position inside the needle were investigated. The designed instrument was exhaustively validated in terms of sensitivity, resolution, and reproducibility by analyzing the standard solutions of methyl isobutyl ketone, heptanone, nonanone, and acetophenone as the test compounds. The results obtained by CD-IMS detector were compared with those of the flame ionization detector, which revealed the capability of the proposed GC-IMS for two-dimensional separation (based on the retention time and drift time information) and identification of an analyte in complex matrixes.

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