title: Quantitative determination of tilmicosin in canine serum by high performance liquid chromatography-tandem mass spectrometry.
abstract: A highly sensitive and quantitative LC/MS/MS assay for the determination of tilmicosin in serum has been developed and validated. For sample preparation, 0.2 mL of canine serum was extracted with 3 mL of methyl tert-butyl ether. The organic layer was transferred to a new vessel and dried under nitrogen. The sample was then reconstituted for analysis by high performance liquid chromatography-tandem mass spectrometry. A Phenomenex Luna C8(2) analytical column was used for the chromatographic separation. The eluent was subsequently introduced to the mass spectrometer by electrospray ionization. A single range was validated for 50-5000 ng/mL for support of toxicokinetic studies. The inter-day relative error (inaccuracy) for the LLOQ samples ranged from -5.5% to 0.3%. The inter-day relative standard deviations (imprecision) at the respective LLOQ levels were < or =10.1%.
authors.affiliation: Elanco Animal Health, A division of Eli Lilly and Co, Greenfield, IN 46140, USA.
authors.forename: Michael
authors.initials: M
authors.lastname: Herrera
authors.forename: Haiqing
authors.initials: H
authors.lastname: Ding
authors.forename: Robert
authors.initials: R
authors.lastname: McClanahan
authors.forename: Jane G
authors.initials: JG
authors.lastname: Owens
authors.forename: Robert P
authors.initials: RP
authors.lastname: Hunter
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004285:Dogs; D004917:Erythromycin / Q000097:blood; D018942:Macrolides / Q000097:blood*; D015394:Molecular Structure; D015588:Observer Variation; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods; D015645:Tylosin / Q000031:analogs & derivatives* / Q000097:blood
chemical_list: D000900:Anti-Bacterial Agents; D018942:Macrolides; D004917:Erythromycin; C052319:tilmicosin; D015645:Tylosin