title: Optimisation by response surface methodology of microextraction by packed sorbent of non steroidal anti-inflammatory drugs and ultra-high performance liquid chromatography analysis of dialyzed samples.
abstract: A procedure based on microextraction by packed sorbent (MEPS) followed by ultra-high performance liquid chromatography (UHPLC) with photodiode array (PDA) detection has been developed for the analysis of seven selected non steroidal anti-inflammatory drugs (NSAIDs) in human dialysates. The influence on MEPS efficiency of pH of the sample, pH of the washing solvent and methanol content in the hydro-alcoholic elution mixture has been investigated by response surface methodology based on a Box-Behnken design of experiments. Among the above factors, pH of sample is the variable that mostly influences MEPS recovery. UHPLC separation of the NSAIDs was completed within less than 4min under isocratic elution conditions on a Fortis SpeedCore C18 column (150×4.6mm I.D., 2.6μm) using acetonitrile-phosphate buffer as the mobile phase. Calibration curves of the NSAIDs were linear over the concentration range 0.025-15μg/mL, with correlation coefficients≥0.998. Intra- and inter-assay relative standard deviations were <8% and recovery values ranged from 94% to 100% for the quality control samples. The results reveal that the developed MEPS/PDA-UHPLC method exhibits a good accuracy and precision and is well suited for the rapid analysis of human dialysate from patients treated with the selected NSAIDs.
authors.affiliation: Dipartimento di Scienze Fisiche e Chimiche, Università degli Studi dell'Aquila, Via Vetoio, 67010 Coppito, L'Aquila, Italy. Electronic address: angeloantonio.darchivio@univaq.it.
authors.forename: Angelo Antonio
authors.initials: AA
authors.lastname: D'Archivio
authors.affiliation: Hortus Novus, Via Collepietro, 67100 L'Aquila, Italy.
authors.forename: Maria Anna
authors.initials: MA
authors.lastname: Maggi
authors.affiliation: Dipartimento di Scienze Fisiche e Chimiche, Università degli Studi dell'Aquila, Via Vetoio, 67010 Coppito, L'Aquila, Italy.
authors.forename: Fabrizio
authors.initials: F
authors.lastname: Ruggieri
authors.affiliation: Dipartimento di Farmacia, Università degli Studi "G. d'Annunzio" Chieti, Pescara, Via dei Vestini, 66100 Chieti, Italy.
authors.forename: Maura
authors.initials: M
authors.lastname: Carlucci
authors.affiliation: Dipartimento di Farmacia, Università degli Studi "G. d'Annunzio" Chieti, Pescara, Via dei Vestini, 66100 Chieti, Italy.
authors.forename: Vincenzo
authors.initials: V
authors.lastname: Ferrone
authors.affiliation: Dipartimento di Farmacia, Università degli Studi "G. d'Annunzio" Chieti, Pescara, Via dei Vestini, 66100 Chieti, Italy.
authors.forename: Giuseppe
authors.initials: G
authors.lastname: Carlucci
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003956:Dialysis; D006863:Hydrogen-Ion Concentration; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013499:Surface Properties
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal
keywords: Dialyzed samples; Microextraction by packed sorbent (MEPS); Non steroidal anti-inflammatory drugs (NSAIDs); Response surface methodology (RSM); Ultra-high performance liquid chromatography (UHPLC) analysis