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

Abstract

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.

Chromatographic determination of biogenic amines in four typical Italian cheeses: correlations with processing and nutritional characteristics through a chemometric approach

“…The determination of BAs is based on ion chromatography coupled with IPAD. This detection technique provides a direct analysis of BA without the need for a derivatization step, and is highly selective, thus improving the already high‐selectivity performance of the chromatographic separation …”

“…This detection technique provides a direct analysis of BA without the need for a derivatization step, and is highly selective, thus improving the already high-selectivity performance of the chromatographic separation. [21][22][23] To elute the seven selected BAs, several isocratic elutions with MSA were tested. At all the investigated MSA concentrations, the observed elution order (ethanolamine, ethylamine, putrescine, cadaverine, histamine, spermidine, and spermine) roughly followed the number of amine groups and hydrophobicity of the molecule.…”

A throughput method using the quick easy cheap effective rugged safe method for the quantification of ibuprofen and its main metabolites in soils

“…Several studies have been published successfully using the QuEChERS method to extract pharmaceuticals from soil samples thus becoming a promising alternative to other extraction methods . The studied therapeutic groups include hormonal steroids , veterinary , nonsteroidal anti‐inflammatory (NSAIDs)/analgesics , psychiatric , and antibiotic drugs . Metabolites were also studied in the works of Bragança et al.…”

“… and de Carlo et al. . In all these publications, commercially available QuEChERS kits from different suppliers were used, which could condition the applicability of the extraction.…”

“…The Quick, Easy, Cheap, Effective, Rugged, and Safe extraction sample preparation method has been widely used since its development and publication by Anastassiades et al in [10][11][12][13] thus becoming a promising alternative to other extraction methods [14][15][16][17]. The studied therapeutic groups include hormonal steroids [10,13,18], veterinary [13,18], nonsteroidal anti-inflammatory (NSAIDs)/analgesics [10,11,13,18], psychiatric [10,12,13,18], and antibiotic drugs [13,18]. Metabolites were also studied in the works of Bragança et al [11] and de Carlo et al [12].…”