Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples
Published Online: Sep 30, 2015
Page range: 345 - 352
Received: Jun 19, 2015
Accepted: Sep 07, 2015
DOI: https://doi.org/10.1515/bvip-2015-0051
Keywords
© 2015 National Veterinary Research Institute in Pulawy
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.
A liquid chromatography – tandem mass spectrometry (LC-MS/MS) method for the determination of oxytetracycline (OTC), 4-epi oxytetracycline (4-epi OTC), tetracycline (TC), 4-epi tetracycline (4-epi TC), chlortetracycline (CTC), 4-epi chlortetracycline (4-epi CTC), doxycycline (DC), minocycline (MINO), methacycline (META) and rolitetracycline (ROLI) residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X) reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% – 103.6%. The decision limits were from 109.0 to 119.8 μg/kg and detection capability varied within the range of 122.2 to 137.6 μg/kg, depending on the analyte.