Determination of siloxanes in water samples employing graphene oxide/Fe3O4 nanocomposite as sorbent for magnetic solid‐phase extraction prior to GC–MS

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Title: Determination of siloxanes in water samples employing graphene oxide/Fe3O4 nanocomposite as sorbent for magnetic solid‐phase extraction prior to GC–MS
Authors: Costa dos Reis, Luciana | Vidal, Lorena | Canals, Antonio
Research Group/s: Espectroscopía Atómica-Masas y Química Analítica en Condiciones Extremas
Center, Department or Service: Universidad de Alicante. Departamento de Química Analítica, Nutrición y Bromatología | Universidad de Alicante. Instituto Universitario de Materiales
Keywords: Gas chromatography with mass spectrometry | Magnetic solid-phase extraction | Nanocomposites | Siloxanes | Water samples
Knowledge Area: Nutrición y Bromatología | Química Analítica
Issue Date: 21-Sep-2018
Publisher: Wiley-VCH Verlag GmbH & Co. KGaA
Citation: Journal of Separation Science. 2018, 41(22): 4177-4184. doi:10.1002/jssc.201800577
Abstract: 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.
Sponsor: The authors would like to thank “Vicerrectorado de Investigación y Transferencia de Conocimiento” of the University of Alicante (UAUSTI16-04), the Ministry of Science and Innovation of Spain (project no. CTQ2011-23968), the Ministry of Economy, Industry and Competitiveness of Spain (project no. CTQ2016-79991-R, AEI/FEDER, UE) for the financial support. L. Costa thanks the Capes Foundation within the Ministry of Education in Brazil (Process 99999.012013/2013-07).
ISSN: 1615-9306 (Print) | 1615-9314 (Online)
DOI: 10.1002/jssc.201800577
Language: eng
Type: info:eu-repo/semantics/article
Rights: © 2018 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim
Peer Review: si
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