Determination of Chloramphenicol Residues in Bee Pollen by Liquid Chromatography/TandemMass Spectrometry

Abstract

Abstract A novel liquid chromatographic/tandem mass spectrometric (LC/MS/MS) method was developed for the trace residue determination of chloramphenicol (CAP) in bee pollen. CAP was extracted from bee pollen with a mixture of methanol and 1 metaphosphoric acid solution, followed by a 2-stage solid-phase extraction enrichment and cleanup. The first stage involved a polymeric cartridge, and the second stage involved an alumina neutral cartridge. The LC separation was performed on a C18 column with 10 mM ammonium formateacetonitrile (7 + 3) as the mobile phase and MS detection with negative-ion electrospray ionization. CAP-d5 was used as the internal standard. The method was validated according to Commission Decision 2002/657/EC. The calibration curves were linear between 0.1 and 5.0 ng/mL, and overall recoveries ranged from 98 to 113. Decision limits (CC) ranged from 0.05 to 0.07 g/kg, and detection capabilities (CC) ranged from 0.08 to 0.12 g/kg. The developed method was applied to 11 samples.