Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry
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Título: | Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry |
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Autor/es: | Cortada Cortés, Carolina | Costa dos Reis, Luciana | Vidal, Lorena | Llorca, Julio | Canals, Antonio |
Grupo/s de investigación o GITE: | Espectroscopía Atómica-Masas y Química Analítica en Condiciones Extremas |
Centro, Departamento o Servicio: | Universidad de Alicante. Departamento de Química Analítica, Nutrición y Bromatología |
Palabras clave: | Volatile siloxanes | Ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) | Experimental design | Wastewater |
Área/s de conocimiento: | Nutrición y Bromatología | Química Analítica |
Fecha de publicación: | 2-dic-2013 |
Editor: | Elsevier |
Cita bibliográfica: | 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 |
Resumen: | A fast, simple and environmentally friendly ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) procedure has been developed to preconcentrate eight cyclic and linear siloxanes from wastewater samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). A two-stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selecting the significant factors involved in the USA-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were: extractant solvent volume, 13 µL; solvent type, chlorobenzene; sample volume, 13 mL; centrifugation speed, 2300 rpm; centrifugation time, 5 min; and sonication time, 2 min. Under the optimized experimental conditions the method gave levels of repeatability with coefficients of variation between 10 and 24% (n=7). Limits of detection were between 0.002 and 1.4 µg L−1. Calculated calibration curves gave high levels of linearity with correlation coefficient values between 0.991 and 0.9997. Finally, the proposed method was applied for the analysis of wastewater samples. Relative recovery values ranged between 71–116% showing that the matrix had a negligible effect upon extraction. To our knowledge, this is the first time that combines LLME and GC-MS for the analysis of methylsiloxanes in wastewater samples. |
Patrocinador/es: | The authors would like to thank the Spanish Ministry of Science and Innovation (project n. CTQ2011-23968), Generalitat Valenciana (Spain) (project n. ACOMP/2013/072) and LABAQUA S.A (Alicante, Spain) for the financial support. |
URI: | http://hdl.handle.net/10045/34544 |
ISSN: | 0039-9140 (Print) | 1873-3573 (Online) |
DOI: | 10.1016/j.talanta.2013.11.042 |
Idioma: | eng |
Tipo: | info:eu-repo/semantics/article |
Revisión científica: | si |
Versión del editor: | http://dx.doi.org/10.1016/j.talanta.2013.11.042 |
Aparece en las colecciones: | INV - SP-BG - Artículos de Revistas |
Archivos en este ítem:
Archivo | Descripción | Tamaño | Formato | |
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2013_Cortada_etal_Talanta.pdf | Accepted Manuscript (acceso abierto) | 602,3 kB | Adobe PDF | Abrir Vista previa |
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