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Magnetic cellulose nanoparticles (MCNPs) were used for the first time as sorbents for stir bar-sorptive dispersive microextraction (SBSDME). The main experimental parameters involved in the SBSDME process that affect extraction (i.e. amount of MCNPs, ionic strength, pH, extraction and back-extraction time) were investigated. The method was applied to the determination of nine polychlorinated biphenyls (PCBs) in fruit juice samples by gas chromatography-mass spectrometry (GC-MS). Under the optimized conditions, a good linearity was obtained in a concentration range of 10-1000 ng mL -1 with determination coefficients over 0.9945. Limits of detection and quantification for all target PCBs were in the range 2.1-54 ng L -1 and 7.0-180 ng L -1 , respectively. Intra-day precision ranged from 1.7% to 8.8% and inter-day precision from 3.4% to 9.3% RSD. The enrichment factors of the analytes were from 74.6 to 98.2. The MCNPs can be reused up to 5 times. The method was applied to commercial orange and pineapple juices (n = 5), where concentrations were below the limits of detection. Recoveries from 70.4 to 108.0% were obtained by applying the method for the analysis of spiked fruit juice samples at 1 and 2 ng mL -1 concentration levels. The use of cellulose makes this approach environmentally friendly and the magnetism of the resulting sorbent in conjunction with SBSDME provides ease of handling and saving of time., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Hybrid nanocomposites based on Fe 3 O 4 magnetic nanoparticles (MNPs) coated with different types of carbon nanotubes (CNTs) have been studied for the first time as sorbent materials for magnetic solid phase extraction (MSPE) for mercury speciation analysis. Monomethylmercury (MMHg) was the target mercury species in water samples and the adsorption and desorption processes were optimized based on this species. Single-walled CNT-MNP showed higher adsorption capacity than double-walled or multi-walled CNTs. Then, the magnetic sorbent was retrieved with an external magnet and MMHg was selectively desorbed from it with dichloromethane (DCM) in two steps with vortex agitation. Inorganic mercury was removed during the desorption stage. The rapid adsorption and desorption equilibrium, the magnetic separation of the sorbent, and the simple and fast synthesis of CNT-MNPs without any additional modification of the CNTs simplified and shortened the extraction procedure. The extract was submitted to derivatization of the mercury species by ethylation (with an optional nitrogen stream evaporation of the organic phase) and injection into a gas chromatograph coupled to an atomic fluorescence detector (GC-pyro-AFS). The overall procedure provides the preconcentration of MMHg up to 150 times and the removal of inorganic mercury at the same time. The procedural limits of detection (LOD) and quantification (LOQ) were 5.4 and 17.9pgmL -1 , respectively. Moreover, magnetic nanocomposites can be reused at least 7 times without losing their efficiency. The methodology was validated in tap, dam and river water samples to evaluate the performance under real conditions with recoveries from 79% to 97% of spiked MMHg., (Copyright © 2017 Elsevier B.V. All rights reserved.)

No previous analytical procedures are available and validated for mercury speciation analysis in terrestrial animal tissues. This analysis is a difficult task both because the expected concentrations are low, since important accumulation process are not likely to occur, and also because there are not commercially available certified reference material. Thus, an analytical methodology has been developed and validated for mercury speciation for the specific case of terrestrial animal tissues. The proposed method is based on the quantitative extraction of the species by closed-vessel microwave assisted heating with an alkaline reagent, followed by ethylation. The ethylated derivatives were then submitted to head-space solid phase microextraction with a 100 μm polidimethylsiloxane-coated fiber, and desorbed onto a gas chromatograph coupled to atomic fluorescence detection via pyrolysis unit (HS-SPME-GC-pyro-AFS). Procedural detection limits were 31.8 ng g(-1) and 52.5 ng g(-1) for CH(3)Hg(+) and Hg(2+), respectively, for liver and 35.3 ng g(-1) and 58.1 ng g(-1) for CH(3)Hg(+) and Hg(2+), respectively, for kidney. These limits of detection are 5.5 and 6 times better than the obtained without solid phase microextraction for CH(3)Hg(+) and Hg(2+), respectively. The methodology was found linear up to 120 μg L(-1) and reproducible from one day to the following. It was validated with certified reference materials NCS ZC 71001 (beef liver) and BCR No 186 (pig kidney) for total mercury, calculated as the sum of species, and with spiked red deer liver and kidney for speciation. Finally, it was applied to the analysis of samples of red deer liver, red deer kidney and wild boar kidney coming from the Almadén's mercury mining area (Ciudad Real, Spain), the longest and largest producer of mercury in the world until its closure in 2002., (Copyright © 2012 Elsevier B.V. All rights reserved.)