An assay to determine rivaroxaban in pharmaceutical formulations by micellar liquid chromatography
- PDF / 658,125 Bytes
- 8 Pages / 595.276 x 790.866 pts Page_size
- 58 Downloads / 185 Views
ORIGINAL PAPER
An assay to determine rivaroxaban in pharmaceutical formulations by micellar liquid chromatography Jaume Albiol‑Chiva1 · Juan Peris‑Vicente2 · Daniel García‑Ferrer2 · Pooja Mishra3 · Priyanka Padhey4 · Devasish Bose4 · Abhilasha Durgbanshi3 · Josep Esteve‑Romero2 Received: 2 January 2020 / Accepted: 22 April 2020 © Iranian Chemical Society 2020
Abstract Rivaroxaban is one of the most prescribed anticoagulants. The ingestion of the correct dosage is a key to the success of the therapy. A procedure to evaluate the content of active principle ingredient in rivaroxaban pharmaceutical formulations, based on micellar liquid chromatography, has been developed. Tablets were solved in the mobile phase and directly injected, thus avoiding the use of large volumes of organic solvents. Analysis was performed using a C18 column and a mobile phase containing 0.05 M sodium dodecyl sulfate—12.5% 1-propanol, buffered at pH 7 with phosphate salt, running under isocratic mode at 1 mL/min. The analyte was resolved in less than 6.0 min. Detection was by UV absorption at 250 nm. The method was successfully validated by the guidelines of the International Conference of Harmonization in terms of specificity, calibration range (0.01–1.00 mg/L), linearity, limit of detection (0.002 mg/L), limit of quantification (0.006 mg/L), trueness (99.6–99.7%), precision ( 98%) were bought from InterQuim (Barcelona, Spain). Sodium dodecyl sulfate (> 99%), dimethyl sulfoxide (DMSO, > 99.6%) and sodium dihydrogen phosphate dihydrate (> 99%) came from Scharlab (Barcelona, Spain). The solvent 1-propanol (HPLC grade) was from Merck (Darmstadt, Germany). Sodium hydroxide (> 98%) was purchased from RiedeldeHaën (Hannover, Germany). Ultrapure water was in-lab produced from deionized water (provided as tap water by the university) using an ultrapure water generator device Simplicity UV (Millipore S.A.S., Molsheim, France). All aqueous solutions were prepared using this water.
Preparation of solutions and mobile phases The micellar solutions were prepared as follows: the proper mass of SDS and NaH2PO4.H2O was solved in ultrapure
Journal of the Iranian Chemical Society
water, and the pH was adjusted by adding drops of NaOH solutions. Then, the adequate volume of the organic solvent was introduced, and the volumetric flask was filled up with ultrapure water. Finally, this solution was ultrasonicated for 5 min to achieve a complete solubilization and filtered through a 0.45 µm-Nylon membrane filters (Micron Separations, Westboro, MA, USA), with the aid of a vacuum pump, to remove solid particles. These solutions were stored in amber bottles at room temperature. A stock solution of rivaroxaban of 100 mg/L was prepared by weighing the appropriate weight and solving it in DMSO. The working solutions were made by successive dilution of the stock solution in mobile phase. These solutions were kept in a fridge at 4 °C.
Chromatographic conditions The chromatographic separation was performed using an HP1100 chromatograph (Agilent Technologies, Palo A
Data Loading...
