Rapid determination of chloramphenicol residues in milk powder by liquid chromatography-elektrospray ionization tandem mass spectrometry

A simple and rapid liquid chromatography tandem mass spectrometry (LC-ESI-MS-MS) confirmation method for the analysis chloramphenicol (CAP) in milk powder has been developed. Samples were extracted by using liquid-iquid extraction steps with ethyl acetate. Lipids were removed using hexsan. LC separation was achieved by using a Phenomenex Luna C-18 column and acetonitryle-water as a mobile phase. The mass spectrometer was operated in multiple reaction monitoring mode (MRM) with negative electro-spray interface (ESI-). The four transitions were monitored m/z 321 -> 257, 321 -> 194, 321 -> 152, 326 -> 157 (IS) and for quantification, the transition m/z 321 -> 152 was chosen. Validation of the method was done according to criteria of Decision Commission No 2002/657 EC. Validation includes the determination of specification, linearity, precision (within- and between-day), accuracy, decision limit (CC(x) and detection capability (CC beta). Samples were fortified at CAP levels 0.30, 0.45 and 0.60 mu g/kg with CAP-5d as internal standard. The precision within-day (RSD%) was lower than 12% and accuracy (RE%) ranged from -9.8 to -3.7%. The precision between-day (RSD%) was less than 15%. The limit of decision (CC alpha) and detection capability (CC beta) for milk powder 0.09 and 0.11 mu g/kg. Value CC alpha and CC beta were calculated for the 321 -> 152 ion transition. This method has been successfully used for routine analysis. (C) 2008 Elsevier B.V. All rights reserved.