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Quantitative determination of rosuvastatin in human plasma by liquid chromatography with electrospray ionization tandem mass spectrometry
Author(s) -
Xu DongHang,
Ruan ZouRong,
Zhou Quan,
Yuan Hong,
Jiang Bo
Publication year - 2006
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2542
Subject(s) - chemistry , chromatography , analyte , selected reaction monitoring , electrospray ionization , liquid chromatography–mass spectrometry , detection limit , formic acid , mass spectrometry , rosuvastatin calcium , tandem mass spectrometry , extraction (chemistry) , analytical chemistry (journal) , rosuvastatin , medicine
A simple and sensitive liquid chromatography/tandem mass spectrometry method was developed and validated for determining rosuvastatin in human plasma, a new synthetic hydroxymethylglutaryl‐coenzyme A reductase inhibitor. The analyte and internal standard (IS; cilostazol) were extracted by simple one‐step liquid/liquid extraction with ether. The organic layer was separated and evaporated under a gentle stream of nitrogen at 40°C. The chromatographic separation was performed on an Atlantis C 18 column (2.1 mm × 150 mm, 5.0 µm) with a mobile phase consisting of 0.2% formic acid/methanol (30:70, v/v) at a flow rate of 0.20 mL/min. The analyses were carried out by multiple reaction monitoring (MRM) using the precursor‐to‐product combinations of m/z 482 → 258 and m/z 370 → 288. The areas of peaks from the analyte and the IS were used for quantification of rosuvastatin. The method was validated according to the FDA guidelines on bioanalytical method validation. Validation results indicated that the lower limit of quantification (LLOQ) was 0.2 ng/mL and the assay exhibited a linear range of 0.2–50.0 ng/mL and gave a correlation coefficient (r ) of 0.9991 or better. Quality control samples (0.4, 8, 25 and 40 ng/mL) in six replicates from three different runs of analysis demonstrated an intra‐assay precision (RSD) 7.97–15.94%, an inter‐assay precision 3.19–15.27%, and an overall accuracy (relative error) of < 3.7%. The method can be applied to pharmacokinetic or bioequivalence studies of rosuvastatin. Copyright © 2006 John Wiley & Sons, Ltd.