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Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

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)...

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Published in:Bulletin of the Veterinary Institute in Puławy 2015-09, Vol.59 (3), p.345-352
Main Authors: Gajda, Anna, Posyniak, Andrzej
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description 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.
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subjects Acetonitrile
Acids
Antibiotics
Chlortetracycline
Chromatography
Doxycycline
Formic acid
Ions
LC-MS/MS
Liquid chromatography
Mass spectrometry
Mass spectroscopy
Methacycline
method validation
Minocycline
Muscles
Oxalic acid
Oxytetracycline
Rolitetracycline
Scientific imaging
Tetracyclines
Trichloroacetic acid
title Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples
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