Sample preparation methods to analyze fipronil in honey by gas chromatography with electron-capture and mass spectrometric detection.
Several sample preparation methods have been assayed to analyze residues of fipronil in honey. After diluting the honey, liquid-liquid extraction (LLE) with organic solvents, and solid-phase extraction (SPE) on commercial cartridges or Florisil-packed column have been tested at three concentration levels: 0.01, 0.1 and 1 mg/kg. LLE with n-hexane or SPE on a Florisil column resulted to be the most suitable procedures to analyze fipronil at trace concentrations. Fipronil was quantified by gas chromatography (GC) with electron-capture detection (ECD) or mass spectrometric (MS) detection after conventional or matrix-matched calibration. The detection limit of fipronil in honey samples was below 1 microg/kg. The degradation of fipronil in honey has also been studied, being identified three minor degradation products in the extracts.
Jiménez
J J
JJ
IU CINQUIMA, Department of Analytical Chemistry, University of Valladolid, Prado de la Magdalena s/n, E-47005 Valladolid, Spain. jjiminez@qua.uva.es
Bernal
J L
JL
del Nozal
Maria J
MJ
Martín
Maria T
MT
Mayo
R
R
D002849:Chromatography, Gas / Q000379:methods*; D006722:Honey / Q000032:analysis*; D007306:Insecticides / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis; D011720:Pyrazoles / Q000032:analysis*; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods
D007306:Insecticides; D010573:Pesticide Residues; D011720:Pyrazoles; C082360:fipronil