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Application of solid-phase microextraction for the determination of pyrethroid residues in vegetable samples by GC-MS

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Abstract

A solid-phase microextraction (SPME) method has been developed for the determination of 7 pyrethroid insecticides (bifenthrin, lambda-cyhalothrin, permethrin, cyfluthrin, cypermethrin, fenvalerate, and tau-fluvalinate) in water, vegetable (tomato), and fruit (strawberry) samples, based on direct immersion mode and subsequent desorption into the injection port of a GC/MS. The SPME procedure showed linear behavior in the range tested (0.5–50 μg L−1 in water and 0.01–0.1 mg kg−1 in tomato) with r 2 values ranging between 0.97 and 0.99. For water samples limits of detection ranged between 0.1 and 2 μg L−1 with relative standard deviations lower than 20%. Detection limits for tomato samples were between 0.003 and 0.025 mg kg−1 with relative standard deviations around 25%. Finally, the SPME procedure has been applied to vegetable (tomato) and fruit (strawberry) samples obtained from an experimental plot treated with lambda-cyhalothrin, and in both cases the analyte was detected and quantified using a calibration curve prepared using blank matrix. SPME has been shown to be a simple extraction technique which has a number of advantages such as solvent-free extraction, simplicity, and compatibility with chromatographic analytical systems. Difficulties with the correct quantification in a complex matrix are also discussed.

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Acknowledgements

This work forms a part of the project entitled "Simplificación de la etapa de preparación de muestra en la determinación de residuos de pesticidas mediante microextracción en fase sólida", developed with the financial support of Fundació Caixa Castelló-Bancaixa 2000.

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Authors and Affiliations

  1. Analytical Chemistry, Experimental Sciences Dept., University Jaume I, P.O. Box 8029 AP, 12080, Castellón, Spain

    J. Beltran, A. Peruga, E. Pitarch, F. J. López & F. Hernández

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  1. J. Beltran
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  2. A. Peruga
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  3. E. Pitarch
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  4. F. J. López
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  5. F. Hernández
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Correspondence to J. Beltran.

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Beltran, J., Peruga, A., Pitarch, E. et al. Application of solid-phase microextraction for the determination of pyrethroid residues in vegetable samples by GC-MS. Anal Bioanal Chem 376, 502–511 (2003). https://doi.org/10.1007/s00216-003-1916-z

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  • DOI: https://doi.org/10.1007/s00216-003-1916-z

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