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-liquid 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 alpha) and detection capability (CC beta). Samples were fortified at CAP levels 0.30, 0.45 and 0.60 microg/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 microg/kg. Value CC alpha and CC beta were calculated for the 321-->152 ion transition. This method has been successfully used for routine analysis.
Rodziewicz
L
L
Department of Hygiene Veterinary, ul. Zwyciestwa 26a, 15-959 Bialystok, Poland. rodziewicz@wiw.bianet.com.pl
Zawadzka
I
I
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis; D002701:Chloramphenicol / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D008892:Milk / Q000737:chemistry*; D011208:Powders; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013997:Time Factors
D000900:Anti-Bacterial Agents; D011208:Powders; D002701:Chloramphenicol