A rapid and sensitive LC-ESI-MS/MS method for detection and quantitation of methylprednisolone and methylprednisolone acetate in rat plasma after intra-articular administration.
作者： Alessia Panusa , Marica Orioli , Giancarlo Aldini , Marina Carini
DOI: 10.1016/J.JPBA.2009.09.041
关键词: Chemistry 、 Protein precipitation 、 Selected reaction monitoring 、 Methylprednisolone acetate 、 Mass spectrometry 、 Formic acid 、 Electrospray 、 Quantitative analysis (chemistry) 、 High-performance liquid chromatography 、 Chromatography
摘要: A rapid, sensitive and specific liquid chromatography-electrospray-tandem mass spectrometric (LC-ESI-MS/MS) method for the simultaneous detection quantitation of methylprednisolone acetate (MPA) (MP) in rat plasma, using a triple-stage quadrupole, has been developed validated. MP-D(2) was used as internal standard (IS) acetonitrile added to plasma samples protein precipitation. After extraction with dichloromethane, analytes were separated on C-12 reversed-phase column by isocratic elution (6min at flow rate 0.2mLmin(-1)) water containing 0.01% formic acid (A) (B) (50:50, v/v). Quantitation performed positive ion multiple reaction monitoring (MRM) mode applying following precursor-to-product transitions: MPA m/z 417-->135+161+253; MP 375-->135+161+253; IS 377-->135+161+253. The method, validated over concentration range 6-600ngmL(-1), shown meet current requirements bioananalytical validation, providing satisfactory results terms linearity, recovery, intra-day inter-day precision accuracy. lower limit (LLOQ) 6ngmL(-1) both (0.080 0.072pmol injected MPA, respectively). successfully applied monitor levels intra-articular (IA) injections low (Depo-Medrol((R))) dose rats.
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