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Microwave assisted headspace single-drop microextration of chlorobenzenes from water samples

Elefteria Psillakis, Claudia E. Domini, Lorena Vidal, Antonio Canals, Nuria Gran

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Περίληψη

Aone-step and in-situ sample preparation method used for quantifying chlorobenzene compounds inwater samples has been developed, couplingmicrowave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto anionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett–Burman screening design wasinitially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionicstrength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions foundfrom this statistical evaluation were: a 5 L microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspaceof a 30mL aqueous sample, irradiated by microwaves at 200W and placed in a 50mL 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 overthe range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, withrelative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low gL−1 range varying between 0.016and 0.039gL−1. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation uponHS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction

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