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Development and validation of automated SPE‐LC‐MS/MS method for determination of indapamide in human whole blood and its application to real study samples
Author(s) -
Nakov N.,
Mladenovska K.,
Labacevski N.,
Dimovski A.,
Petkovska R.,
Dimitrovska A.,
Kavrakovski Z.
Publication year - 2013
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.2957
Subject(s) - chromatography , chemistry , indapamide , electrospray ionization , selected reaction monitoring , mass spectrometry , bioanalysis , ammonium formate , extraction (chemistry) , tandem mass spectrometry , analytical chemistry (journal) , diuretic , medicine , endocrinology
A fast and simple liquid chromatography–electrospray ionization tandem mass spectrometry method for determination of indapamide in human whole blood was developed and validated. The sample extraction of indapamide from human whole blood was achieved using automated solid‐phase extraction. Chromatographic separation was performed on Kinetex C 18 column (100 × 2.1 mm, 1.7 µm particle size) using acetonitrile and 2 m m ammonium formate in ratio 90:10 (v/v) as a mobile phase. The mass spectrometer was operated in the multiple reaction monitoring mode using positive electrospray ionization for indapamide and the internal standard (zolpidem tartarate). The total run time was 2.5 min. The present method was found to be linear in the concentration range of 1–50 ng/mL with the coefficient of determination 0.9987. The absolute recoveries of indapamide were 90.51–93.90%. The method was validated according the recommendations for validation of bioanalytical methods of European Medicines Agency guideline and was successfully used to analyze human whole blood samples for application in a pharmacokinetic study. Copyright © 2013 John Wiley & Sons, Ltd.