Determination of chloramphenicol residues in bee pollen by liquid chromatography/tandem mass spectrometry.
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 formate-acetonitrile (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 (CCalpha) ranged from 0.05 to 0.07 microg/kg, and detection capabilities (CCbeta) ranged from 0.08 to 0.12 microg/kg. The developed method was applied to 11 samples.
Fujita
Kazuhiro
K
Japan Food Research Laboratories, 7-4-41, Saitoasagi, Ibaraki-shi, Osaka 567-0085, Japan. fujitak@jfrl.or.jp
Ito
Hironobu
H
Nakamura
Munetomo
M
Watai
Masatoshi
M
Taniguchi
Makoto
M
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001516:Bees; D002138:Calibration; D002701:Chloramphenicol / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis*; D007202:Indicators and Reagents; D011058:Pollen / Q000737:chemistry*; D015203:Reproducibility of Results; D012996:Solutions; D053719:Tandem Mass Spectrometry
D000900:Anti-Bacterial Agents; D007202:Indicators and Reagents; D012996:Solutions; D002701:Chloramphenicol