A fast, simple, economical, and environmentally friendly magnetic solidphase extraction (MSPE) procedure has been developed to preconcentrate 2,4,6-trinitrotoluene (TNT) from water samples prior to determination by liquid chromatography-UV-Vis employing graphene oxide/Fe O nanocomposite as sorbent. The nanocomposite synthesis was investigated, and the MSPE was optimized by a multivariate approach. The optimum MSPE conditions were: 40 mg of nanocomposite, 10 min of vortex extraction, 1 mL of acetonitrile as eluent, and 6 min of desorption in an ultrasonic bath. Under the optimized experimental conditions, the method was evaluated obtaining a preconcentration factor of 153. The linearity of the method was studied from 1 to 100 µg L (N!=!5), obtaining a correlation coefficient of 0.994. The relative standard deviation and limit of detection This is a previous version of the article published in Analytical and Bioanalytical Chemistry. 2017, 409(10): 2665-2674. doi:10.1007 were found to be 12% (n!=!6, 10 µg L ) and 0.3 µg L , respectively. The applicability of the method was investigated, analyzing three types of water samples (i.e., reservoir and drinking water and effluent wastewater) and recovery values ranged between 87 and 120% (50 µg L spiking level) showing that the matrix had a negligible effect upon extraction. Finally, the semiquantitative Eco-Scale metrics confirmed the greenness of the developed method.
Cite this article as: Carol Cortada, Luciana Costa dos Reis, Lorena Vidal, Julio Llorca, Antonio Canals, Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry, Talanta, http: //dx.doi. org/10.1016/j.talanta.2013.11.042 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting galley proof before it is published in its final citable form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.
A new, fast, simple, and environmentally friendly analytical method has been developed to determine six siloxanes in water samples: octamethyltrisiloxane, octamethylcyclotetrasiloxane, decamethyltetrasiloxane, decamethylcyclopentasiloxane, dodecamethylpentasiloxane and dodecamethylcyclohexasiloxane. The analytical method consists of magnetic solid‐phase extraction employing graphene oxide/Fe3O4 as sorbent for the separation and preconcentration of siloxanes prior to GC–MS determination. The extraction procedure was optimized by means of a Plackett‐Burman design. Under the optimized extraction conditions (graphene oxide/Fe3O4, 20 mg; extraction time, 10 min; eluent volume, 0.5 mL ACN; elution time, 2.5 min; sample volume, 20 mL), the method rendered repeatability levels with a relative standard deviation between 9 and 20% (n = 6, 10 μg/L). Methodological limits of detection ranged from 0.003 to 0.1 μg/L. The linearity of the method was studied between the methodological limit of quantification and 100 μg/L, obtaining correlation coefficient values between 0.990 and 0.999. The applicability of the method was assessed by analyzing drinking, river and wastewater samples. Relative recovery values ranged between 70 and 120% (1 and 60 μg/L spiking level) showing that the matrix had a negligible effect on extraction. Finally, the greenness of this method was confirmed by the semiquantitative Eco‐Scale metrics.
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