Dispersive solid-phase extraction followed by dispersive liquid–liquid microextraction for the determination of some sulfonylurea herbicides in soil by high-performance liquid chromatography

Abstract

Dispersive solid-phase extraction (DSPE) combined with dispersive liquid–liquid microextraction (DLLME) has been developed as a new approach for the extraction of four sulfonylurea herbicides (metsulfuron-methyl, chlorsulfuron, bensulfuron-methyl and chlorimuron-ethyl) in soil prior to high-performance liquid chromatography with diode array detection (HPLC-DAD). In the DSPE-DLLME, sulfonylurea herbicides were first extracted from soil sample into acetone–0.15 mol L −1 NaHCO 3 (2:8, v/v). The clean-up of the extract by DSPE was carried out by directly adding C 18 sorbent into the extract solution, followed by shaking and filtration. After the pH of the filtrate was adjusted to 2.0 with 2 mol L −1 HCl, 60.0 μL chlorobenzene (as extraction solvent) was added into 5.0 mL of it for DLLME procedure (the acetone contained in the solution also acted as dispersive solvent). Under the optimum conditions, the enrichment factors for the compounds were in the range between 102 and 216. The linearity of the method was in the range from 5.0 to 200 ng g −1 with the correlation coefficients ( r) ranging from 0.9967 to 0.9987. The method detection limits were 0.5–1.2 ng g −1. The relative standard deviations varied from 5.2% to 7.2% ( n = 5). The relative recoveries of the four sulfonylurea herbicides from soil samples at spiking levels of 6.0, 20.0 and 60.0 ng g −1 were in the range between 76.3% and 92.5%. The proposed method has been successfully applied to the analysis of the four target sulfonylurea herbicides in soil samples, and a satisfactory result was obtained.