Rapid and sensitive determination of two degradation products of flumethrin in honey by ultrasonically assisted extraction and gas chromatography with electron capture detection

J Sep Sci. 2007 Aug;30(12):1912-9. doi: 10.1002/jssc.200700023.

Abstract

A rapid and sensitive method for the determination of 4-fluoro-3-phenoxybenzaldehyde cyanohydrin (FPBC) and 4-fluoro-3-phenoxy-benzaldehyde (FPB) in honey samples using ultrasonically assisted extraction and gas chromatography with electron capture detection (GC-ECD) has been developed. The different factors affecting the efficiency of the extraction were carefully optimized. The honey sample was extracted with a mixture of hexane and dichloromethane (v/v, 1:1) utilizing the ultrasonically assisted technique and cleaned up by solid-phase extraction on Oasis HLB cartridges. The eluate was evaporated to dryness and residues were reconstituted to 1.0 mL with hexane and determined by GC-ECD. The calibration curves of fortified samples showed acceptable linear response (R(2) >0.99) over a range of 3-100 ng/g for FPBC and FPB in seven replicate determinations of six concentrations, respectively, and analysis of variance (ANOVA) with a lack-of-fit test was performed to validate the regression data. Overall average recoveries ranged from 90.9 to 106.2% for honey samples. The detection limits were 0.9 ng/g for FPBC and 1.0 ng/g for FPB, respectively. This method can be successfully applied to routine determination of two degradation products of flumethrin in honey samples.

MeSH terms

  • Acetone / analysis
  • Benzaldehydes / chemistry*
  • Chemistry Techniques, Analytical / methods
  • Chromatography, Gas / methods*
  • Electrons
  • Hexanes / analysis
  • Honey
  • Methylene Chloride / analysis
  • Models, Chemical
  • Nitriles / chemistry*
  • Plant Extracts / chemistry
  • Pyrethrins / analysis
  • Pyrethrins / chemistry*
  • Pyrethrins / isolation & purification
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Solvents

Substances

  • Benzaldehydes
  • Hexanes
  • Nitriles
  • Plant Extracts
  • Pyrethrins
  • Solvents
  • cyanohydrin
  • Acetone
  • flumethrin
  • Methylene Chloride