Determination of alachlor, metolachlor, and their acidic metabolites in soils by microwave-assisted extraction (MAE) combined with solid phase extraction (SPE) coupled with GC-MS and HPLC-UV analysis

Abstract

A well-validated analytical method based on microwave-assisted extraction (MAE) and SPE is presented for the combined analysis of alachlor, alachlor–oxanilic acid (OXA), alachlor–ethanesulfonic acid (ESA), metolachlor, metolachlor–OXA, metolachlor–ESA residues in soils. Extraction of solutes by soil sample was carried out by MAE for 20 min at 100°C in the presence of 50 mL solution (methanol/water 50:50), the extract was subsequently passed through C18 cartidges and fractionated into two fractions, the first with parent compounds (PCs) analyzed with GC-MS and the second one containing the metabolites analyzed with HPLC. For the SPE step, various types of sorbents (Environmental C18, tC18, Supelclean ENVI-carb, and LiChrolut EN) have been used, and their respective advantages and disadvantages are discussed. After the method optimization, average recovery values of all solutes were > 71% in the 50–500 μg/kg fortification range with RSD <10%. The LOQ and LOD were 10–50 and 5–10 μg/kg, respectively. The method was validated with two types of soils (1 and 2.4% organic matter) and in fresh (12 h aging), intermediate (1 wk aging), and aged (1 month aging) spiked samples. Moreover, residue levels determined after field application of alachlor or metolachlor were higher when soils were processed using this method than with a comparison method based on an overnight flask shaking (FS) of soil suspension.