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In the present study, nano-sized titanium oxides were applied for preconcentration and determination of Pb(II) in aqueous samples using hollow fiber based solid-liquid phase microextraction (HF-SLPME) combined with flame atomic absorption spectrometry (FAAS). In this work, the nanoparticles dispersed in caprylic acid as an extraction solvent was placed into a polypropylene porous hollow fiber segment supported by capillary forces and sonification. This membrane was in direct contact with solutions containing Pb (II). The effect of experimental conditions on the extraction, such as pH, stirring rate, sample volume, and extraction time were optimized. Under the optimal conditions, the performance of the proposed method was investigated for the determination of Pb (II) in food and water samples. The method was linear in the range of 0.6-3000μgmL -1 . The relative standard deviations and relative recovery of Pb (II) was 4.9% and 99.3%, respectively (n=5)., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

A new design of hollow fiber solid-liquid phase microextraction (HF-SLPME) was developed for the determination of benzodiazepines (BZPs) in hair, urine and wastewater. The membrane extraction with 1-pentyl-3-methylimidazolium bromide coated titanium dioxide ([PMIM]Br@TiO2) sorbent used in this research is a two-phase supported membrane extraction consisting of an aqueous (donor phase), and n-octanol/nano [PMIM]Br@TiO2 (acceptor phase) system operated in direct immersion sampling mode. The 1-pentyl-3-methylimidazolium bromide (ionic liquid) coated nano TiO2 dispersed in the organic solvent (n-octanol) is held into a porous membrane supported by capillary forces and sonification. It is in contact with the feed phase, which is the aqueous sample. The experimental setup is very simple and highly affordable. The hollow fiber is disposable, so single use of the fiber reduces the risk of cross-contamination and carry-over problems. The proposed method allows the very effective and enriched recuperation of BZPs into one single extract. In order to obtain high extraction efficiency of the analytes using this novel sorbent, the main parameters were optimized. Under the optimized extraction conditions, the method showed good linearity (0.05-6000ngmL(-1)), low limits of detection (0.08-0.5ngmL(-1)) and good enrichment (533-1190)., (Copyright © 2014 Elsevier B.V. All rights reserved.)

A polyvinylimidazole/sol-gel composite is proposed as a novel solid-phase microextraction fiber to extract five halobenzenes from the headspace of aqueous solutions in combination with gas chromatography with mass spectrometry. The prepared fiber was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The obtained results showed that porous polyvinylimidazole/sol-gel composite was chemically deposited on fused silica fiber. The effect of important extraction parameters including extraction temperature, extraction time, and salt content were investigated. The optimum conditions were as follows: extraction temperature 25°C, extraction time 20 min, and salt concentration 30 w/v%. Detection limits and relative standard deviations of the developed method for halogenated benzenes were below 0.1 pg/mL and 15%, respectively. Repeatability of the proposed method, explained by relative standard deviation, varied between 5.48 and 9.15% (n = 5). The limits of detection (S/N = 3) ranged between 0.01 and 0.10 ng/L using gas chromatography with mass spectrometry with selected ion monitoring mode. For real sample analysis, three types of water samples with different matrices (ground, surface, and tap water) were studied. The optimized procedure was applied to extraction and method validation of halogenated benzenes in spiked water samples., (© 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)