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Matrix solid-phase dispersion extraction of organophosphorus pesticides from propolis extracts and recovery evaluation by GC/MS

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Abstract

Five organophosphorus pesticides (dichlorvos, diazinon, malathion, methyl parathion and coumaphos) were extracted from propolis by matrix solid-phase dispersion (MSPD) extraction using octadecylsilica (C18, 1.0 g) as dispersant material. The kind of solvent elution (acetonitrile or ethyl acetate), volume (8 mL and 15 mL), and adsorbent used to clean-up the extracts (graphitized carbon, florisil™ and silica) were optimized using fortified propolis samples (5.0 μg g−1). Recovery was determined by gas chromatography with mass spectrometric detection in selected ion monitoring mode (GC/MS-SIM) and statistical analysis was done to determine better extraction conditions. Relatively high recovery and lower relative standard deviation values (3.1–14.6%) were obtained when analytes were eluted with ethyl acetate from the MSPD column. Diazinon, malathion, methyl parathion, and coumaphos show recoveries of 72.7%, 84.6%, 62.6%, and 78.3%, respectively. In contrast, the recovery for dichlorvos was 53.8%. Additional adsorbents tested for clean-up and increase in solvent elution did not affect recoveries positively and caused a high background in chromatograms. Thus, final conditions were 1 mL of sample, 1 g C18 and 8 mL of ethyl acetate.

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Acknowledgments

This work has been carried out with financial support from CONACyT-SAGARPA-COFUPRO-2005 [project: 12699]. The authors thank Mrs. Maria Guadalupe Palafox Hernandez for manuscript revision.

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Authors and Affiliations

  1. Facultad de Ingeniería Química, Universidad Autónoma de Yucatán, Periférico Norte Km. 33.5, Tablaje catastral 13615, Colonia Chuburná de Hidalgo Inn, C.P. 97203, Mérida, Yucatán, Mexico

    Gloria M. Acosta-Tejada & David Muñoz-Rodríguez

  2. Facultad de Matemáticas, Universidad Autónoma de Yucatán, Periférico Norte Km. 33.5, Tablaje catastral 13615, Apartado Postal 172, Cordemex, C.P. 97110, Mérida, Yucatán, Mexico

    Salvador Medina-Peralta

  3. Instituto Nacional de Investigaciones Forestales, Agrícolas y Pecuarias, CE Mocochá, km. 25 carretera Mérida-Motul, Mérida, C.P. 97454, Mocochá, Yucatán, Mexico

    Yolanda B. Moguel-Ordóñez

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  1. Gloria M. Acosta-Tejada
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  2. Salvador Medina-Peralta
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  3. Yolanda B. Moguel-Ordóñez
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  4. David Muñoz-Rodríguez
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Correspondence to David Muñoz-Rodríguez.

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Acosta-Tejada, G.M., Medina-Peralta, S., Moguel-Ordóñez, Y.B. et al. Matrix solid-phase dispersion extraction of organophosphorus pesticides from propolis extracts and recovery evaluation by GC/MS. Anal Bioanal Chem 400, 885–891 (2011). https://doi.org/10.1007/s00216-011-4828-3

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