Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples |
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Authors: | Vidal Lorena Domini Claudia E Grané Nuria Psillakis Elefteria Canals Antonio |
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Institution: | a Departamento de Química Analítica, Nutrición y Bromatología, Universidad de Alicante, P.O. Box 99, E-03080 Alicante, Spain b Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Crete, Greece |
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Abstract: | A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 μL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low μg L−1 range varying between 0.016 and 0.039 μg L−1. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction. |
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Keywords: | Chlorinated aromatic compounds Microwave-assisted Liquid phase microextraction Ionic liquid Experimental design Water analysis Sample pretreatment |
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