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Seven quick, easy, cheap, effective, rugged and safe (QuEChERS)-based procedures, differing in both the extraction and clean-up steps, were investigated for the recovery of bentazone (BTZ), atrazine (ATZ), carbamazepine (CBZ), phenytoin (PNT) and its metabolite 5-(p-hydroxyphenyl-),5-phenylhydantoin (HPPH) from soil. Target analytes were chosen for their extensive use and/or occurrence in soil, as well as for their medium-high polarity characteristics (log K OW values in the range 0.88-2.80), which have been reported as a critical parameter for the recovery from soil with QuEChERS approaches. Liquid chromatography coupled with UV and pulsed amperometric (PA) detection at a glassy carbon electrode was used as instrumental technique. The recovery data obtained within each tested procedure were discussed for each compound investigated, highlighting different behaviour depending on the specific physicochemical characteristics of the analytes. The optimized QuEChERS conditions consisted of the extraction of analytes with CH3CN:H2O 70:30, 5 % CH3COOH, followed by a dispersive solid-phase extraction (d-SPE) clean-up step with C18 sorbent. This method, in which water is directly added to the soil together with acetonitrile and salts, allowed the rehydration step to be avoided, which can be as long as 30 min. Matrix effects were evaluated for both the detection techniques at different concentration levels, and they were below 24 % for both the detection technique used. The recoveries were evaluated at three concentration levels by a matrix-matched calibration and were in the ranges of 83-113 % (relative standard deviations (RSD) ≤ 14 %) and 88-109 % (RSD ≤ 11 %) for UV and PA detection, respectively, highlighting very good performances of the method, even for the more polar analytes. Method detection limits ranged from 4 μg/kg (BTZ) to 493 μg/kg (PNT) and from 4 μg/kg (HPPH) to 11 μg/kg (BTZ) for UV and PA detection, respectively. The method was finally compared with a microwave-assisted extraction procedure which provided less satisfactory extraction performances than the optimized QuEChERS procedure.

analytical and bioanalytical chemistry

Evaluation of different QuEChERS procedures for the recovery of selected drugs and herbicides from soil using LC coupled with UV and pulsed amperometry for their detection