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      MSPD procedure for determining buprofezin, tetradifon, vinclozolin, and bifenthrin residues in propolis by gas chromatography-mass spectrometry.

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          Abstract

          A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine bifenthrin, buprofezin, tetradifon, and vinclozolin in propolis using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). Different method conditions were evaluated, for example type of solid phase (C(18), alumina, silica, and Florisil), the amount of solid phase and eluent (n-hexane, dichloromethane, dichloromethane-n-hexane (8:2 and 1:1, v/v) and dichloromethane-ethyl acetate (9:1, 8:2 and 7:3, v/v)). The best results were obtained using 0.5 g propolis, 1.0 g silica as dispersant sorbent, 1.0 g Florisil as clean-up sorbent, and dichloromethane-ethyl acetate (9:1, v/v) as eluting solvent. The method was validated by analysis of propolis samples fortified at different concentration levels (0.25 to 1.0 mg kg(-1)). Average recoveries (four replicates) ranged from 67% to 175% with relative standard deviation between 5.6% and 12.1%. Detection and quantification limits ranged from 0.05 to 0.10 mg kg(-1) and 0.15 to 0.25 mg kg(-1) propolis, respectively.

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          Author and article information

          Journal
          Anal Bioanal Chem
          Analytical and bioanalytical chemistry
          Springer Nature America, Inc
          1618-2650
          1618-2642
          Mar 2008
          : 390
          : 5
          Affiliations
          [1 ] Departamento de Química, Universidade Federal de Sergipe, Av. Marechal Rondon s/no, Jardim Rosa Elze, Cep. 49100-000, São Cristóvão, SE, Brazil.
          Article
          10.1007/s00216-007-1813-y
          18193409

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