Multiresidue pesticides analysis in soils using modified QuEChERS with disposable pipette extraction and dispersive solid-phase extraction

• Published in: Journal of separation science 2013-01, Vol.36 (2), p.376-382
• Main Authors: Fernandes, Virgínia C., Domingues, Valentina F., Mateus, Nuno, Delerue-Matos, Cristina
• Format: Article
• Language: English
• Subjects: Analysis methods; Analytical chemistry; Applied sciences; Calibration; Chemistry; Chromatographic methods and physical methods associated with chromatography; Dispersive solid-phase extraction; Disposable pipette extraction; Exact sciences and technology; Gas chromatographic methods; Gas chromatography tandem mass spectrometry; Gas Chromatography-Mass Spectrometry; Integrated pest management; Limit of Detection; Liquid-liquid extraction; Liquid-Liquid Extraction - methods; Organic farming; Pesticide Residues - analysis; Pesticide Residues - isolation & purification; Pesticides; Pests; Pipettes; Pollution; Recovery; Separation; Soil and sediments pollution; Soil contamination; Soil Pollutants - analysis; Soil Pollutants - isolation & purification; Soils; Solid Phase Extraction - instrumentation; Solid Phase Extraction - methods
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201200673

QuEChERS original method was modified into a new version for pesticides determination in soils. The QuEChERS method is based on liquid–liquid portioning with ACN and was followed by cleanup step using dispersive SPE and disposable pipette tips. Gas chromatographic separation with MS detection was carried out for pesticides quantification. The method was validated using recovery experiments for 36 multiclass pesticides. Mean reco‐veries of pesticides at each of the four spiking levels between 10–300 μg/kg of soil ranged from 70–120% for 26 pesticides with RSD values less than 15%. The method achieved low limit of detection less than 7.6 μg/kg. Matrix effects were observed for 13 pesticides. Matrix effects were compensated by using matrix‐matched calibration. The method was applied successfully using d‐SPE or DPX in the analysis of the pesticides in soils from organic farming and integrated pest management.