Headspace solvent microextraction-gas chromatographic thermionic specific detector determination of amitraz in honey after hydrolysis to 2,4-dimethylaniline

Abstract

A novel headspace solvent microextraction (HSME) method for the extraction of trace amounts of 2,4-dimethylaniline (2,4-DMA), produced after hydrolysis of amitraz, is presented. The hydrolysis reaction and HSME were carried out in a single step, and then the preconcentrated 2,4-DMA was analyzed gas chromatographically using a thermionic specific detector (TSD). Different parameters affecting the HSME procedure including the type of solvent, headspace volume, stirring rate, Na 2SO 4 content, solution and microdrop temperature, drop volume and extraction time were studied and optimized. The optimized conditions were 25 min solution equilibrium time, 10 min solvent equilibrium time, 5 mL headspace volume, 600 rpm stirring rate, 15% Na 2SO 4, solution temperature 60 °C, microdrop temperature 4 °C and microdrop volume 3 μL. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 10 and 30 ng amitraz g −1 honey, respectively, and the dynamic linear range was from 0.03 to 10 μg amitraz g −1 honey. Finally, the proposed method was applied to the quantification of amitraz in spiked honey samples. Because of performing hydrolysis and extraction processes in a single step, the method provided a rapid, simple and sensitive approach to analysis of amitraz.