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Analytical Utility of Quadrupole Time-of-Flight Mass Spectrometry for the Determination of Pesticide Residues in Comparison with an Optimized Column High-Performance Liquid Chromatography/Tandem Mass Spectrometry Method

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A multiresidue method for the analysis of 30 pesticides with different physicochemical properties in fruits and vegetables was developed. The method involves a rapid and small-scale extraction procedure based on matrix solid-phase dispersion using octadecylsilyl (C18) as the dispersant and dichloromethane as the eluent. The target pesticides were determined using column high-performance liquid chromatography/triple quadrupole-tandem mass spectrometry (LC/QqQ-MS/MS). The method was validated for sensitivity, linearity, reproducibility, and accuracy. A recovery study was conducted at 3 different levels, and the average ranged from 74 to 99 for all of the studied compounds, with relative standard deviations lower than 19. The proposed method achieved limits of quantitation between 0.5 and 10 g/kg, well below the maximum residue limits. The capability of the extraction procedure to extract pesticide residues other than those selected as target analytes has been checked by ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/QqTOF-MS). Four incurred pesticides, not covered in the method as target analytes, were identified and unequivocally confirmed. Both systems were demonstrated to be complementary. LC/QqQ-MS/MS has the advantage that its detection limits are somewhat lower, and UPLC/QqTOF-MS offers the possibility to identify pesticides and transformation products not included as targets of the study.
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Document Type: Research Article

Affiliations: 1: Universitat de Valncia, Facultat de Farmcia, Laboratori de Nutrici i Bromatologia, Av. Vicent Andrs Estells s/n, 46100 Burjassot, Valncia, Spain. 2: Instituto de Diagnstico Ambiental y Estudios del Agua-Consejo Superior de Investigaciones Cientifcas, Department of Environmental Chemistry, c/ Jordi Girona, 18-26, 08034 Barcelona, Spain. 3: Instituto de Diagnstico Ambiental y Estudios del Agua-Consejo Superior de Investigaciones Cientifcas, Department of Environmental Chemistry, c/ Jordi Girona, 18-26, 08034 Barcelona, Spain and Catalan Institute for Water Research (ICRA) c/ Pic de Peguera, 15, 17003 Girona, Spain.

Publication date: 28 May 2009

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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