Rapid Determination of Chloramphenicol Residues in Honey by Liquid Chromatography Tandem Mass Spectrometry and the Validation of Method Based on 2002/657/EC
L Rodziewicz, Iwona Zawadzka
Abstract
L Rodziewicz, Iwona Zawadzka
Abstract
A simple and rapid liquid chromatography tandem mass spectrometry (LCMS/MS) method of analysis for the chloramphenicol (CAP) in honey was developed. Samples were cleaned-up with hexane and followed extraction with acetonitrile. LC separation was achieved by using a Phenomenex Luna C-18 column and acetonitrile – water as a mobile phase. The mass spectrometer was carried out in a multiple reaction monitoring mode with negative electrospray interface. Validation of the method was done according to criteria of Decision Commission No 2002/657 EC. Samples were fortified at CAP levels between 0.15 and 0.45 μg/kg with CAP-5d as internal standard. The precision within-day was lower than 9% and recovery was in the range of 91-104%. The limit of decision (CCα) and detection capability (CCβ) were 0.11μg/kg and 0.14 μg/kg, respectively. The validation method was successfully applied for determination of CAP in honey.
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A simple and rapid liquid chromatography tandem mass spectrometry (LCMS/MS) method of analysis for the chloramphenicol (CAP) in honey was developed. Samples were cleaned-up with hexane and followed extraction with acetonitrile. LC separation was achieved by using a Phenomenex Luna C-18 column and acetonitrile – water as a mobile phase. The mass spectrometer was carried out in a multiple reaction monitoring mode with negative electrospray interface. Validation of the method was done according to criteria of Decision Commission No 2002/657 EC. Samples were fortified at CAP levels between 0.15 and 0.45 μg/kg with CAP-5d as internal standard. The precision within-day was lower than 9% and recovery was in the range of 91-104%. The limit of decision (CCα) and detection capability (CCβ) were 0.11μg/kg and 0.14 μg/kg, respectively. The validation method was successfully applied for determination of CAP in honey.
Key concepts: Chromatography, Chemistry, Mass spectrometry, Liquid chromatography–mass spectrometry, Extraction (chemistry), Tandem mass spectrometry, Electrospray, Detection limit