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Development of a sensitive method for simultaneous determination of fluticasone propionate and salmeterol in plasma samples by liquid chromatography‐tandem mass spectrometry
Author(s) -
Silvestro Luigi,
Savu Simona Rizea,
Savu Simoicoleta,
Tudoroniu Ariana,
Tarcomnicu Isabela
Publication year - 2012
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.1708
Subject(s) - chemistry , chromatography , salmeterol , extraction (chemistry) , mass spectrometry , electrospray , tandem mass spectrometry , electrospray ionization , matrix (chemical analysis) , fluticasone , sample preparation , liquid chromatography–mass spectrometry , fluticasone propionate , detection limit , analytical chemistry (journal) , corticosteroid , medicine , surgery , asthma
A new method for the fast simultaneous quantification of fluticasone propionate and salmeterol from plasma samples by liquid chromatography–tandem mass spectrometry, with adequate sensitivity for pharmacokinetic applications, was developed and validated. The chromatographic separation and mass‐spectrometric parameters were optimized for the retention and detection of the two compounds, despite quite different structures and properties. Two columns connected in series were used, cation‐exchange (Zorbax 300‐SCX, 5 cm × 2.1 mm, 5 µm) and octadecyl (Discovery HSC 18 , 10 cm × 2.1 mm, 5 µm). The mass‐spectrometric interface was operated in negative electrospray ionization mode; high sensitivity and lesser matrix effects were obtained, permitting smaller consumption of plasma. The sample preparation was based on supported liquid–liquid extraction in 96‐well format plates that provided clean samples with a simplified procedure that was suitable for automation. The method was validated according to regulatory guidelines, by assessing lower limits of quantification, selectivity, linearity, accuracy, precision, extraction recoveries and matrix effects. A comparison with two other methods for the separate determination of fluticasone propionate and salmeterol in plasma samples, previously developed by our group, is presented. The statistical evaluation of the results obtained with the three methods on a set of unknown samples from treated patients demonstrated good correlation ( R 2 0.987 for fluticasone propionate and 0.967 for salmeterol). Copyright © 2011 John Wiley & Sons, Ltd.