Determination of chloramphenicol in honey by liquid chromatography–tandem mass spectrometry

Abstract

An effective liquid chromatographic method with tandem mass spectrometric (LC–MS/MS) detection and identification is presented for the determination of chloramphenicol (CAP) in honey. After a preliminary dissolution in water, samples were extracted with a mixture of dichloromethane/acetone and evaporated to dryness; the following clean up was carried out on an octadecyl (C₁₈) SPE cartridge. CAP was determined by LC–MS/MS, using electrospray ionization in the negative ion mode (ESI⁻). The column was a LUNA Phenomenex with a mixture of methanol-aqueous ammonium acetate (60:40, v/v) as a mobile phase. Honey samples were fortified at CAP levels 0.30–0.45–0.60 μg kg⁻¹ with 5D-CAP as internal standard. At these levels, trueness ranged between 98.7 and 102.0% and within-laboratory reproducibility was lower than 6.2%, expressed as relative standard deviation. The limit of decision (CCα) was 0.07 μg kg⁻¹ and detection capability (CCβ) was 0.10 μg kg⁻¹.