The present study reports the development and validation of a stability indicating assay method for clofarabine in injection on a UPC 2 Ô (ultra performance convergence chromatography) instrument, which utilizes the unrealized potential of supercritical fluid chromatography. The use of UPC 2 Ô provides a single viable technique that is a sustainable, reduced cost, and green technology that lowers the use of organic solvents. Based on this advantage, we explored a simple and robust method in order to increase sample throughput and productivity to quantify clofarabine in the presence of its potential impurities and other degradants. The separation was achieved on a BEH-2-ethyl pyridine (BEH 2EP) column (100 mm  3.0 mm I.D. with an average pore diameter of 1.7 mm) by using methanol as a cosolvent and carbon dioxide as a mobile phase in the ratio of 30 : 70. The detection is carried out at a wavelength of 254 nm. We are able to achieve the separation of clofarabine from its potential impurities and other degradants in less than 6 minutes with a low amount of solvent consumption. The new method is validated in accordance with the ICH-guidelines and exhibited good intra-and inter-day precision, accuracy and linearity (r 2 $ 0.999) over a range of 50% to 150% of target concentration.
In the present study total twelve impurities of Bisoprolol (BISO) and Hydrochlorothiazide (HCTZ) were separated simultaneously in a single HPLC method. Out of these 12 impurities, five are potential degradants, which are validated as per ICH guidelines. As the two active drug substances BISO and HCTZ have different solubilities and polarities, the most critical parameters in resolving the components from each other are pH, temperature, and solvents. The method is precise (RSD<1.0%), accurate, linear (r 2 >0.999), robust, and stability indicating in the range of LOQ to 150%. The HPLC method is then migrated to UPLC to further reduce the, run time, solvent consumption, and increase the sample through put.
In the present study, supercritical fluid (carbon dioxide) chromatographic methods were developed and validated for the quantitative assay determination of two cancer therapeutic substances, fulvestrant and azacitidine, using a UPC2 system. Fulvestrant was separated from six potential impurities, while impurities of azacitidine were separated using a 150 mm  4.6 mm, I.D., a chiral column and 5 mm, particle size. Both drugs were analysed simultaneously in a single sequence using multiple channels in the system and respective methods. These new methods were validated for their intended purpose in accordance with the current ICH guidelines. The method exhibited excellent intra-and inter-day precision. A precision with RSD 1% and 1.6% was achieved for fulvestrant and azacitidine, respectively. A linear relationship r 2 > 0.999 was achieved between the concentration and detector response over a range of 25-150% of the target concentrations for both compounds. The two compounds were well quantified from their unspecified impurities obtained from stress studies. The method can be employed for routine quality control testing and stability analysis.
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