Journal
ANALYTICA CHIMICA ACTA
Volume 529, Issue 1-2, Pages 257-263Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2004.10.059
Keywords
chloramphenicol; honey; solid-phase extraction; liquid chromatography-tandem mass spectrometry; validation
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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 (C-18) 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 mug 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 (CCalpha) was 0.07 mug kg(-1) and detection capability (CCbeta) was 0.10 mug kg(-1). (C) 2004 Elsevier B.V. All rights reserved.
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