A simple, fast and cost-effective liquid chromatographic/tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of flunixin 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. Flunixin detection was performed with positive electrospray ionization in Selected Reaction Monitoring (SRM) mode, monitoring one precursor and two products ions. For quantification purposes, flunixin-d3 was used as internal standard. The matrix effect on the analysis of flunixin 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). Flunixin stability was also investigated in matrix and in sample extracts at different times and storage conditions.

A quick LC-MS/MS method for determination of flunixin in bovine muscle

LUGOBONI, BARBARA;BARBAROSSA, ANDREA;GAZZOTTI, TERESA;ZIRONI, ELISA;FARABEGOLI, FEDERICA;PAGLIUCA, GIAMPIERO
2014

Abstract

A simple, fast and cost-effective liquid chromatographic/tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of flunixin 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. Flunixin detection was performed with positive electrospray ionization in Selected Reaction Monitoring (SRM) mode, monitoring one precursor and two products ions. For quantification purposes, flunixin-d3 was used as internal standard. The matrix effect on the analysis of flunixin 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). Flunixin stability was also investigated in matrix and in sample extracts at different times and storage conditions.
Barbara Lugoboni; Andrea Barbarossa; Teresa Gazzotti; Elisa Zironi; Federica Farabegoli; Giampiero Pagliuca
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11585/190552
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