Ultrasound-assisted extraction followed by liquid chromatography coupled to tandem mass spectrometry for the simultaneous determination of multiclass herbicides in soil

• Published in: Analytical and bioanalytical chemistry 2023-12, Vol.415 (29-30), p.7197-7209
• Main Authors: Castiñeira-Landeira, Ana, Vazquez, Lua, Gonzalez-Leirado, Helena, Llompart, María, Dagnac, Thierry
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Bentazone; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatography; Chromatography, High Pressure Liquid - methods; Chromatography, Liquid - methods; Design of experiments; Design optimization; Environmental protection; Experimental design; Food Science; Herbicides; Herbicides - analysis; Laboratory Medicine; Liquid chromatography; Mass spectrometry; Mass spectroscopy; Methanol; Methodology; Metolachlor; Monitoring/Environmental Analysis; Organic soils; Pendimethalin; Research Paper; Room temperature; Scientific imaging; Soil; Soil analysis; Soil contamination; Soils; Solid Phase Extraction; Solvent extraction; Solvents; Solvents - analysis; Tandem Mass Spectrometry - methods; Ultrasonic imaging; Ultrasonic testing; Ultrasound; Water - analysis
• ISSN: 1618-2642; 1618-2650; 1618-2650
• DOI: 10.1007/s00216-023-04987-y

An analytical methodology based on ultrasound-assisted extraction (UAE) followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) has been developed for the identification and quantification of 9 authorized herbicides in soil (dimethenamid-P, imazamox, S-metolachlor, nicosulfuron, pendimethalin, prosulfuron, bentazone, terbuthylazine, and mesotrione). Preliminary experiments dealing with solvent extraction, the extraction technique, and herbicide response comparison in soil, with and without organic amendments, were carried out with the purpose of obtaining high sample throughput and sensitivity. UAE and the solvent mixture water:methanol demonstrated higher efficiency and they were selected as sample treatment and extraction solvent, respectively. Critical parameters affecting UAE were optimized by experimental design. In the present research, the extraction technique used in the official EPA microwave-assisted extraction (MAE) methodology (United States Environmental Protection Agency) and UAE optimized methodology were compared. The results indicated that the developed method showed better efficacy since microwave extraction gave very poor responses for nicosulfuron and prosulfuron. The temperature extraction was also optimized; room temperature was the most suitable to work with. Under the optimized conditions, the proposed UAE-LC-MS/MS method was assessed in terms of linearity ( R 2  ≥ 0.9912), accuracy (recoveries around 100%), and precision (relative standard deviation, RSD