title: Determination of fluvalinate residues in beeswax by gas chromatography with electron-capture detection.
abstract: A simple, rapid, and accurate method is described for the determination of residual fluvalinate in beeswax. The procedure consists of partitioning on a disposable column of diatomaceous earth (Extrelut), followed by chromatographic cleanup on a Florisil cartridge. The final extract is analyzed by capillary gas chromatography with electron-capture detection (GC-ECD). Briefly, wax samples were dissolved in n-hexane, and the solutions were sonicated and transferred to Extrelut columns. The fluvalinate was extracted with acetonitrile, and a portion of the extract was cleaned up on a Florisil cartridge. The fluvalinate was eluted with diethyl ether-n-hexane (1 + 1) and directly determined by GC-ECD. Recoveries from wax samples spiked at 5 fortification levels (100-1500 microg/kg) ranged from 77.4 to 87.3%, with coefficients of variation of 5.12-8.31%. The overall recovery of the method was 81.4 +/- 3.2%, and the limit of determination was 100 microg/kg.
authors.affiliation: National Agricultural Research Foundation, Institute of Veterinary Research of Athens, Laboratory of Honey Analysis, Greece.
authors.forename: A
authors.initials: A
authors.lastname: Tsigouri
authors.forename: U
authors.initials: U
authors.lastname: Menkissoglu-Spiroudi
authors.forename: A T
authors.initials: AT
authors.lastname: Thrasyvoulou
authors.forename: G C
authors.initials: GC
authors.lastname: Diamantidis
mesh_terms: D002138:Calibration; D002849:Chromatography, Gas; D004563:Electrochemistry; D007202:Indicators and Reagents; D007306:Insecticides / Q000032:analysis*; D009570:Nitriles; D010573:Pesticide Residues / Q000032:analysis*; D011722:Pyrethrins / Q000032:analysis*; D014885:Waxes / Q000737:chemistry*
chemical_list: D007202:Indicators and Reagents; D007306:Insecticides; D009570:Nitriles; D010573:Pesticide Residues; D011722:Pyrethrins; D014885:Waxes; C038228:beeswax; C034227:fluvalinate