In:
Current Pharmaceutical Analysis, Bentham Science Publishers Ltd., Vol. 15, No. 4 ( 2019-03-19), p. 305-311
Abstract:
Rivaroxaban is the first oral, selective direct FXa inhibitor with rapid onset of
action and its biological toxicity may be related to the enantiomer. 〈 /P 〉 〈 P 〉 Objective: The aim of the current study was to develop and validate a precise, accurate, and specific
direct Chiral-RP-UPLC-MS/MS method for the enantiomeric separation and detection of rivaroxaban and its enantiomer. Methods: The present study screened various conditions of chromatographic and mass spectra, including
chromatographic column model, flow velocity, phase ratio, column temperature, and collision energy, parent/daughter ion pairs, etc. Try to match the chromatographic and mass spectrometric conditions. Results: Good Rs (Rs 〉 2.5) was achieved on a Chiralpak IC column (4.6 × 250 mm, 5µm) using
H2O:acetonitrile (10:90) as mobile phase at 25 oC column temperature. The rate of flow was set at 0.4 ml/min and enantiomers were detected by triple-quadruple tandem mass spectrometry using positive
electrospray ionization (ESI) with MRM transitions of m/z 436.07 〉 144.95. The cone voltage and collision
energy were kept at 48 V and 28 eV, respectively. The limit of detection and quantification of (S)- rivaroxaban were 0.39 and 1.30 ng/ml, respectively. This method was validated and found to be selective,
precise, accurate, linear and robust for the quantitative determination of chiral impurities. It is also a good application for the blood samples analysis in vitro. Conclusion: Chiral-RP-UPLC-MS/MS method has entirely detected (S)-rivaroxaban and its (R)- enantiomer
in very low concentration and complex matrix directly, especially for blood samples.
Type of Medium:
Online Resource
ISSN:
1573-4129
DOI:
10.2174/1573412914666180409145403
Language:
English
Publisher:
Bentham Science Publishers Ltd.
Publication Date:
2019
SSG:
15,3
