Pesticidi i Fitomedicina (Jan 2012)
Comparison of Methods for Bifenthrin Residues Determination in Fermented Wheat Samples
Abstract
Efficiency of three different sample preparation methods for GC/MS determinationof bifenthrin residues in wheat (Triticum spelta) samples fermented by Lactobacillusplantarum was tested. The first method was based on a methanol:acetone=1:1 extractionfolowed by a purification on columns containing mixture of aluminium oxide and activatedcharcoal slurry-packed and eluted with dichlormethane, the second was based onmethanol:acetone=1:1 extraction folowed by the purification on florisil column and elutionby ethil acetate:acetone=4:1, while the third tested method was based on a combinationof the first two mentioned methods, thus methanol:acetone=1:1 extraction and clean-upthrought columns filled with a mixture of aluminum oxide and activated charcoal slurrypackedand eluted with ethil acetate:acetone=4:1. The second method was the most effectivefor obtaining satisfactory recoveries for bifenthrin in a range of 79-83% for four fortificationlevels, with good reproducibility i.e. RSD% in a range of 2.2-7.4%. The chosen methodwas further optimized by assessing the optimum volume of elution solvent used duringthe clean-up procedures. The highest recovery of 82.1% was obtained after elution with25 ml of solvent. Overall, two-step extraction with 25 ml of methanol:acetone=1:1 solventmix for 30 min, followed by clean-up procedure through a glass column with florisil coupledwith elution with 25 ml of ethyl acetate: acetone=4:1, allows simple, efficient and reliableGC/MS detection of bifenthrin residues from wheat grain fermented by L. plantarum.
