Evaluation of solid-phase microextraction conditions for the determination of chlorophenols in honey samples using gas chromatography

Abstract

A rapid and solvent-free method for the determination of nine chlorophenol (CP) compounds in honey samples using headspace solid-phase microextraction (HS–SPME) and gas chromatography with atomic emission detection (GC–AED) is developed. The different factors affecting the efficiency of the extraction and derivatization steps were carefully optimized. The polydimethylsiloxane–divinylbenzene (PDMS/DVB) fiber was the most suitable for preconcentrating the analytes from the headspace of an aqueous solution containing the dissolved honey samples where the chlorophenols had been submitted to acetylation. When the matrix effect was evaluated for different samples, it was concluded that standard addition calibration was required for quantification purposes. Detection limits roughly ranged from 0.1 to 2.4 ng g −1, depending on the compound and the honey sample analyzed, with a fiber time exposure of only 15 min at 75 °C. The optimized method was successfully applied to different samples, some of the studied chlorophenols being detected in some of the analyzed honeys at concentration levels 0.6–9.4 ng g −1.