Dispersive suspended microextraction

A novel sample pre-treatment technique termed dispersive suspended microextraction (DSME) coupled with gas chromatography-flame photometric detection (GC-FPD) has been developed for the determination of eight organophosphorus pesticides (ethoprophos, malathion, chlorpyrifos, isocarbophos, methidathion, fenamiphos, profenofos, triazophos) in aqueous samples. In this method, both extraction and two phases’ separation process were performed by the assistance of magnetic stirring. After separating the two phases, 1 μL of the suspended phase was injected into GC for further instrument analysis. Varieties of experiment factors which could affect the experiment results were optimized and the following were selected: 12.0 μL p-xylene was selected as extraction solvent, extraction speed was 1200 rpm, extraction time was 30 s, the restoration speed was 800 rpm, the restoration time was 8 min, and no salt was added. Under the optimum conditions, limits of detections (LODs) varied between 0.01 and 0.05 μg L⁻¹. The relative standard deviation (RSDs, n = 6) ranged from 4.6% to 12.1%. The linearity was obtained by five points in the concentration range of 0.1–100.0 μg L⁻¹. Correlation coefficients (r) varied from 0.9964 to 0.9995. The enrichment factors (EFs) were between 206 and 243. In the final experiment, the developed method has been successfully applied to the determination of organophosphorus pesticides in wine and tap water samples and the obtained recoveries were between 83.8% and 101.3%. Compared with other pre-treatment methods, DSME has its own features and could achieve satisfied results for the analysis of trace components in complicated matrices.