title: A quick LC-MS-MS method for the determination of flunixin in bovine muscle.
abstract: A simple, fast and cost-effective liquid chromatographic/tandem mass spectrometry (LC-MS-MS) method for the quantitative determination of flunixin (FLU) in bovine muscle was developed and validated. The sample preparation procedure involved an extraction with acetonitrile, followed by evaporation and reconstitution. Chromatographic separation was achieved on a reverse-phase column under programmed conditions. FLU detection was performed with positive electrospray ionization in selected reaction monitoringmode, monitoring one precursor and two products ions. For quantification purposes, FLU-d3 was used as an internal standard. The matrix effect on the analysis of FLU in bovine muscle was evaluated by comparison between calibration curves prepared with standard solution and in blank matrix extracts. The equivalent responses obtained confirmed the absence of signal suppression or/and enhancement. The method was extensively validated according to the parameters requested by European Commission Decision 2002/657/EC in terms of specificity, limit of detection, linearity, trueness, precision, decision limit (CCα) and detection capability (CCβ). FLU stability was also investigated in matrix and in sample extracts at different times and storage conditions.
authors.affiliation: 1 VETSPIN SRL, Via Tolara di Sopra, 50 I 40064 Ozzano dell'Emilia, Bologna, Italy.
authors.forename: B
authors.initials: B
authors.lastname: Lugoboni
authors.forename: A
authors.initials: A
authors.lastname: Barbarossa
authors.forename: T
authors.initials: T
authors.lastname: Gazzotti
authors.forename: E
authors.initials: E
authors.lastname: Zironi
authors.forename: F
authors.initials: F
authors.lastname: Farabegoli
authors.forename: G
authors.initials: G
authors.lastname: Pagliuca
mesh_terms: D000818:Animals; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D002138:Calibration; D002417:Cattle; D002853:Chromatography, Liquid / Q000592:standards; D003002:Clonixin / Q000031:analogs & derivatives* / Q000032:analysis; D004355:Drug Stability; D057230:Limit of Detection; D018482:Muscle, Skeletal / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000592:standards; D053719:Tandem Mass Spectrometry / Q000592:standards; D013997:Time Factors
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; C014557:flunixin; D003002:Clonixin