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Headspace single-drop microextraction for the analysis of chlorobenzenes in water samples

Vidal Lorena , Canals Antonio, Kalogerakis Nikos, Psyllaki Eleftheria

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Περίληψη

Exposing a microlitre organic solvent drop to the headspace of an aqueous sample contaminated with ten chlorobenzene compounds proved to be an excellent preconcentration method for headspace analysis by gas chromatography–mass spectrometry (GC–MS). The proposed headspace single-drop microextraction (SDME) method was initially optimised and the optimum experimental conditions found were: 2.5 μl toluene microdrop exposed for 5 min to the headspace of a 10 ml aqueous sample containing 30% (w/v) NaCl placed in 15 ml vial and stirred at 1000 rpm. The calculated calibration curves gave a high level of linearity for all target analytes with correlation coefficients ranging between 0.9901 and 0.9971, except for hexachlorobenzene where the correlation coefficient was found to be 0.9886. The repeatability of the proposed method, expressed as relative standard deviation varied between 2.1 and 13.2% (n = 5). The limits of detection ranged between 0.003 and 0.031 μg/l using GC–MS with selective ion monitoring. Analysis of spiked tap and well water samples revealed that matrix had little effect on extraction. A comparative study was performed between the proposed method, headspace solid-phase microextraction (SPME), solid-phase extraction (SPE) and EPA method 8121. Overall, headspace SDME proved to be a rapid, simple and sensitive technique for the analysis of chlorobenzenes in water samples, representing an excellent alternative to traditional and other, recently introduced, methods.

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