PMID- 30780011 OWN - NLM STAT- MEDLINE DCOM- 20190318 LR - 20190318 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1110-1111 DP - 2019 Mar 15 TI - Determination of the total tulathromycin residues in bovine muscle, fat, and liver by liquid chromatography-tandem mass spectrometry. PG - 51-58 LID - S1570-0232(18)31672-6 [pii] LID - 10.1016/j.jchromb.2019.02.011 [doi] AB - A reliable and accurate liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based method was developed to quantify total tulathromycin residues in bovine tissues. Specifically, the above method relied on the quantification of CP-60,300, a marker produced by tulathromycin hydrolysis, for which maximum residue limits (MRLs) were established by the European Union and several other countries. Sample preparation and LC-MS/MS conditions were thoroughly optimized to allow for accurate quantification. The optimized procedure involved sample homogenization with 2 mol/L hydrochloric acid and ethyl acetate, heating of the resulting aqueous layer to convert tulathromycin and its metabolites into the marker residue, cleanup by a polymer-based cation-exchange cartridge, and subsequent analysis by LC-MS/MS. The developed method was validated for tulathromycin A and the marker residue in bovine muscle, fat, and liver at two levels, namely at the MRL set in Japan and at 0.01 mg/kg. Excellent analytical performance was observed, with the average recoveries of tulathromycin A and the marker residue ranging from 98 to 107%, and relative standard deviations ranging from 1 to 3%. Matrix effects were negligible, and analyte loss during sample preparation was minimal for all matrices tested, which allowed for accurate determination by external standard calibration using a solvent standard. No interfering peaks were observed close to the retention time of the marker residue for all matrices, which was indicative of high specificity. Overall, the developed method was proven suitable for regulatory purpose analysis of total tulathromycin residues. CI - Copyright (c) 2019 Elsevier B.V. All rights reserved. FAU - Saito-Shida, Shizuka AU - Saito-Shida S AD - Division of Foods, National Institute of Health Sciences, Tonomachi 3-25-26, Kawasaki-ku, Kawasaki, Kanagawa 210-9501, Japan. Electronic address: shizsaito@nihs.go.jp. FAU - Kashiwabara, Nao AU - Kashiwabara N AD - Division of Foods, National Institute of Health Sciences, Tonomachi 3-25-26, Kawasaki-ku, Kawasaki, Kanagawa 210-9501, Japan. FAU - Nemoto, Satoru AU - Nemoto S AD - Division of Foods, National Institute of Health Sciences, Tonomachi 3-25-26, Kawasaki-ku, Kawasaki, Kanagawa 210-9501, Japan. FAU - Akiyama, Hiroshi AU - Akiyama H AD - Division of Foods, National Institute of Health Sciences, Tonomachi 3-25-26, Kawasaki-ku, Kawasaki, Kanagawa 210-9501, Japan. LA - eng PT - Journal Article DEP - 20190212 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Disaccharides) RN - 0 (Heterocyclic Compounds) RN - Q839I13422 (tulathromycin) SB - IM MH - Adipose Tissue/chemistry MH - Animals MH - Cattle MH - Chromatography, Liquid/*methods MH - Disaccharides/*analysis/pharmacokinetics MH - Drug Residues/*analysis/pharmacokinetics MH - Heterocyclic Compounds/*analysis/pharmacokinetics MH - Limit of Detection MH - Linear Models MH - Liver/*chemistry MH - Muscle, Skeletal/*chemistry MH - Reproducibility of Results MH - Tandem Mass Spectrometry/*methods MH - Tissue Distribution OTO - NOTNLM OT - Bovine tissue OT - Hydrolysis OT - LC-MS/MS OT - Tulathromycin EDAT- 2019/02/20 06:00 MHDA- 2019/03/19 06:00 CRDT- 2019/02/20 06:00 PHST- 2018/11/06 00:00 [received] PHST- 2019/01/19 00:00 [revised] PHST- 2019/02/10 00:00 [accepted] PHST- 2019/02/20 06:00 [pubmed] PHST- 2019/03/19 06:00 [medline] PHST- 2019/02/20 06:00 [entrez] AID - S1570-0232(18)31672-6 [pii] AID - 10.1016/j.jchromb.2019.02.011 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Mar 15;1110-1111:51-58. doi: 10.1016/j.jchromb.2019.02.011. Epub 2019 Feb 12.