A new, simple, sensitive and specific liquid chromatography/electrospray ionization tandem mass spectrometric (LC/ESI-MS/MS) method in precursor ion scanning (PIS) mode has been developed for the rapid detection of methylprednisolone acetate (MPA) and its metabolites in rat urine. A suitable product ion specific for methylprednisolone (MP) and MPA was selected after a fragmentation study on 20 (cortico)steroids at different collision energies (5-40 eV). Urine samples were simply treated with acetonitrile then dried in a SpeedVac system. The method was validated and compared with other PIS methods for detecting corticosteroids in human urine. It was more sensitive, with limit of detection (LOD) and lower limit of quantitation (LLOQ), respectively, of 5 and 10 ng mL-1. The method was applied for the analysis of rat urine collected before and after (24, 48, 72 h) intra-articular (IA) injection of a marketed formulation of MPA (Depo-Medrol®). MS/MS acquisitions were taken at different collision energies for the precursor ions of interest, detected in PIS mode, to verify the MP-related structure. Six different metabolites were detected in rat urine, and their chemical structures were assigned with a computational study.

A sensitive and specific precursor ion scanning approach in liquid chromatography/electrospray ionization tandem mass spectrometry to detect methylprednisolone acetate and its metabolites in rat urine / A. Panusa, G. Aldini, M. Orioli, G. Vistoli, G. Rossoni, M. Carini. - In: RAPID COMMUNICATIONS IN MASS SPECTROMETRY. - ISSN 0951-4198. - 24:11(2010), pp. 1583-1594. [10.1002/rcm.4555]

A sensitive and specific precursor ion scanning approach in liquid chromatography/electrospray ionization tandem mass spectrometry to detect methylprednisolone acetate and its metabolites in rat urine

A. Panusa
Primo
;
G. Aldini
Secondo
;
M. Orioli;G. Vistoli;G. Rossoni
Penultimo
;
M. Carini
Ultimo
2010

Abstract

A new, simple, sensitive and specific liquid chromatography/electrospray ionization tandem mass spectrometric (LC/ESI-MS/MS) method in precursor ion scanning (PIS) mode has been developed for the rapid detection of methylprednisolone acetate (MPA) and its metabolites in rat urine. A suitable product ion specific for methylprednisolone (MP) and MPA was selected after a fragmentation study on 20 (cortico)steroids at different collision energies (5-40 eV). Urine samples were simply treated with acetonitrile then dried in a SpeedVac system. The method was validated and compared with other PIS methods for detecting corticosteroids in human urine. It was more sensitive, with limit of detection (LOD) and lower limit of quantitation (LLOQ), respectively, of 5 and 10 ng mL-1. The method was applied for the analysis of rat urine collected before and after (24, 48, 72 h) intra-articular (IA) injection of a marketed formulation of MPA (Depo-Medrol®). MS/MS acquisitions were taken at different collision energies for the precursor ions of interest, detected in PIS mode, to verify the MP-related structure. Six different metabolites were detected in rat urine, and their chemical structures were assigned with a computational study.
Settore CHIM/08 - Chimica Farmaceutica
2010
Article (author)
File in questo prodotto:
Non ci sono file associati a questo prodotto.
Pubblicazioni consigliate

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/2434/143853
Citazioni
  • ???jsp.display-item.citation.pmc??? 1
  • Scopus 14
  • ???jsp.display-item.citation.isi??? 15
social impact