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Sample Preparation Based on Matrix Solid-Phase Dispersion and Solid-Phase Extraction Cleanup for the Determination of Organochlorine Pesticides in Fish

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A method based on matrix solid-phase dispersion (MSPD) and SPE to determine 20 organochlorine pesticides (OCPs) in fish tissues (muscle and liver) was optimized in terms of the sorbents and elution solvents used for the analysis. The following analytical components were evaluated: ENVI-Carb and ENVI-18 as dispersing agents, Florisil and Florisil over alumina as cleanup adsorbents, and hexane and hexaneethyl acetate (80 + 20) as elution solvents. The pesticides were determined by GC with electron capture detection. The best results were obtained with ENVI-Carb as a dispersing agent and an ENVI-Florisil co-column using 40 mL hexaneethyl acetate (80 + 20) as the elution solvent. Analytical recoveries ranged between 75 and 130 except for -HCH in fish liver, and the RSD values were <15 for most of the pesticides studied. Furthermore, sensitivity was sufficient (LOD of <300 g/kg) for all OCPs under study, in compliance with the tolerance limits of the U.S. Food and Drug Administration for OCPs in fish. The results were compared with those obtained by microwave-assisted extraction (MAE) and pressurized liquid extraction (PLE) in order to evaluate the performance of the MSPD procedure. The MPSD methodology was shown to be easy to use and fast, with a clear advantage relative to cost, because it does not need the expensive equipment required for MAE and PLE.
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Document Type: Research Article

Affiliations: University of A Corua, Department of Analytical Chemistry, Campus da Zapateira, s/n, E-15071, A Corua, Spain; Instituto Universitario de Medioambiente, Pazo de Lngora, Lins, Oleiros, E-15179, A Corua, Spain.

Publication date: May 1, 2010

More about this publication?
  • 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 The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better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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