Abstract
A stability-indicating reversed phase ultra performance liquid chromatographic (RP-UPLC) method was developed for the determination of related substances in rosuvastatin calcium (ROSV) tablet dosage form. The chromatographic separation was achieved on an Acquity BEH C18 (100 mm × 2.1 mm, 1.7 μm) column with mobile phase containing a gradient mixture of solvent-A (0.1% trifluoroacetic acid) and solvent-B (methanol). The eluted compounds were monitored at 240 nm and the run time was 10.0 min. Degradation behavior of the ROSV was studied under various degradation stress conditions. Four major unknown degradation products (late eluting impurities) were found in acid stress condition and two unknown degradation products were found in oxidative stress condition. The developed method separates (six) unknown impurities, (three) known impurities and ROSV substance from each other, providing the stability-indicating power of the method. The developed RP-UPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. The developed and validated RP-UPLC method is LC-MS compatible and can be applied for identification of eluted unknown impurities of ROSV.
Highlights
Rosuvastatin (ROSV) is a synthetic lipid-lowering agent, chemically known as (3R,5S,6E)7-{4-(4-fluorophenyl)-6-(1-methylethyl)-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl}-3,5dihydroxyhept-6-enoic acid calcium salt (2:1)
A detailed literature survey for ROSV revealed that few analytical methods were reported for determination of ROSV by HP-TLC [2], UV spectroscopy [3,4,5,6], assay by RP-HPLC [7,8,9,10,11], capillary electrophoresis [12], Mass spectrometry [13,14,15,16], LC-MS/MS [17] and simultaneous determination with atorvastatin by mass spectrometry [18]
A spiked solution of impurities (5 μg/mL), ROSV (500 μg/mL) and placebo peaks were subjected to separation by reversed phase ultra performance liquid chromatographic (RP-UPLC)
Summary
Rosuvastatin (ROSV) is a synthetic lipid-lowering agent, chemically known as (3R,5S,6E)7-{4-(4-fluorophenyl)-6-(1-methylethyl)-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl}-3,5dihydroxyhept-6-enoic acid calcium salt (2:1) It is used for the treatment of hyperlipidemia and is an inhibitor of 3-hydroxy-3-methylglutaryl coenzyme (HMG-CoA) reductase. Mehta et al reported a stability-indicating assay method for determination of ROSV in the presence of its degradation products using high performance liquid chromatography [19] In this assay method total run time is around 35 min to elute all degradation impurities and is applicable for only ROSV estimation but not for its related substances. We focused on developing a selective, fast, cost-effective, mass compatible and stability-indicating method using advance technique UPLC for the related substances determination of ROSV in solid pharmaceutical dosage form. Thereafter, the developed method was successfully validated according to International Conference on Harmonization (ICH) guidelines [21] to show the stabilityindicating capability of the method
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