Comparison of several extraction procedures for the determination of biopesticides in soil samples by ultrahigh pressure LC-MS/MS

• Published in: Journal of separation science Vol. 35; no. 7; pp. 861 - 868
• Main Authors: Prestes, Osmar D., Padilla-Sánchez, Juan Antonio, Romero-González, Roberto, Grio, Sergio López, Frenich, Antonia Garrido, Martínez-Vidal, José Luis
• Format: Journal Article
• Language: English
• Published: Weinheim Blackwell Publishing Ltd 01.04.2012; Wiley
• Subjects: Agricultural soils; Analysis methods; Analytical chemistry; Applied sciences; Biopesticides; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Cleaning; Exact sciences and technology; Extraction; Liquids; Methyl alcohol; Modified QuEChERS extraction; Nicotine; Organic agriculture; Other chromatographic methods; Pesticide Residues - analysis; Pesticide Residues - isolation & purification; Pollution; Recovery; Residues; Soil (material); Soil and sediments pollution; Soil Pollutants - analysis; Soil Pollutants - isolation & purification; Solid Phase Extraction - methods; Tandem Mass Spectrometry - methods; UHPLC-MS/MS; Tandem mass spectrometry; Chemical analysis; Agricultural soils; Modified QuEChERS extraction; HPLC chromatography; Solvent extraction; Soil pollution; Electrospray; Chemical enrichment; Dispersive Solid-Phase Extraction; Sample preparation; QuEChERS; Biopesticides; Biopesticide; Quantitative analysis; Trace analysis; Validation; Coupled method; Agricultural soil; Operating conditions; Reversed phase chromatography; UHPLC-MS/MS; Organic agriculture; Extraction method; Comparative study
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201101057

A new procedure has been proposed for the determination of biopesticides (nicotine, sabadine, veratridine, rotenone, azadirachtin, cevadine, deguelin, spynosad D, and pyrethrins) and piperonyl butoxide in agricultural soils. Several extraction procedures such as solid–liquid extraction using mechanical shaking, sonication, pressurized liquid extraction, and modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) have been tested, obtaining better results when QuEChERS procedure without further cleanup steps was applied. The determination of the compounds was carried out by ultra high pressure liquid chromatography coupled to tandem mass spectrometry, using methanol and aqueous solution of ammonium formate 5 mM as mobile phase. The method was validated for all compounds at concentrations ranging from 10 to 100 μg/kg and recoveries ranged from 68 to 116%, except for nicotine and sabadine, with recoveries lower than 50%. Precision was estimated through intra‐ and inter‐day studies, obtaining intra‐day precision lower than 20% for most of the compounds, and inter‐day precision was lower than 25%. Limits of detection and quantification were also estimated, obtaining limits of quantification equal or lower than 10 μg/kg. Finally, the method was applied to the analysis of 20 real agricultural soil samples and no biopesticide residues were found over the limit of quantification.