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A green HPLC method for the determination of apixaban in pharmaceutical products: Development and validation

Abstract Apixaban (APX) is a novel anticoagulant drug used in the treatment of ischemic stroke and venous thromboembolism. In this study, two different chromatographic methods were developed for the determination of APX in pharmaceutical products. In the first method, an Agilent C18 column (250 mm × 4.6 mm, 5 μm) was used, and the temperature was kept constant at 30°C. The mobile phase was chosen to be 0.1% trifluoroacetic acid solution and acetonitrile (65:35, v/v), and isocratic elution was applied. The flow rate of the mobile phase was found to be 1.0 mL·min−1 and the injection volume was 20 µL. The detection was carried out at a wavelength of 276 nm using a UV detector. In the second method, ethanol was used as an organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated in accordance with ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1 of APX. Later, these chromatographic methods were applied to tablet formulations. Comparison of the obtained results in terms of mean was made using Student’s (t) test, and comparisons in terms of standard deviations were made using the Fisher (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using AGREE-Analytical greenness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of APX in pharmaceutical formulations.

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Canagliflozin: A review with specific focus on analytical methods in biological matrices and pharmaceuticals

Abstract Sodium-glucose transporter 2 inhibitor emerges as the latest group of oral hypoglycemic agents, which shows insulin-independent pathology and provides an upper hand to enhance renal glucose elimination. Canagliflozin (CGN) was the number one drug, approved by FDA on 29th March 2013 for the treatment of type 2 diabetes mellitus. By totting up to its glucose-lowering effects, it exhibits beneficial effects on the heart and potentially on the kidneys. The study aims to summarize various analytical techniques, such as chromatography, spectrophotometry, and hyphenated techniques, such as Liquid chromatography with tandem mass spectrometry (LC-MS/MS) and Ultra performance liquid chromatography with tandem mass spectrometer (UPLC-MS) for the analysis of CGN. In the proposed work, we have reviewed various analytical methods reported for the estimation of CGN in biological matrices and Pharmaceuticals from various databases like ScienceDirect, Springer, PubMed, Scopus, Taylor & Francis, and Web of Science for the estimation of CGN. Various analytical methods adapted were high-performance liquid chromatography, UPLC, LC-MS/MS, high-performance thin-layer liquid chromatography, Fourier-transform infrared spectroscopy, spectrofluorimetry, and UV spectrophotometry. This current review presented the determination of CGN using various analytical techniques and biological matrices either in single or in combination with other hypoglycemic agents, as per International Conference on Harmonization guidelines. Further, some future trends that can be integrated were also suggested.

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Purification and characterisation of phytochemicals extracted from <i>Rhizophora mucronata</i>: Their efficacy against <i>Pseudomonas aeruginosa</i> infection in <i>Catla catla</i>

Abstract The aim of this work is to purify and characterise bioactive molecules from various solvent extracts prepared with the leaves of Rhizophora mucronata, a mangrove plant. In vitro assessment of antibacterial activity of n-hexane, diethyl ether, ethanol, and aqueous extracts (AEs) against Bacillus subtilis (0.4 ± 0.1, 1.1 ± 0.3, 0.9 ± 0.1, and 1.2 ± 0.7 mm), Staphylococcus aureus (1.2 ± 0.1, 2.3 ± 0.5, 3.2 ± 1.2, and 4.4 ± 1.7 mm), Klebsiella pneumoniae (0.5 ± 0.3, 1.7 ± 0.4, 3.9 ± 1.4, and 3.9 ± 0.9 mm), and Pseudomonas aeruginosa (0.2 ± 0.1, 2.5 ± 0.6, 3.7 ± 0.5, and 4.2 ± 1.3 mm) has proven to act as potent similar to that of commercial antibiotic. Corresponding to antibacterial activity result, antioxidant activity was also higher for AE (75.97% ± 0.5%) compared to remaining extracts (73.77% ± 2.5%, 69.99% ± 0.4%, and 65.24% ± 1.8%) at a concentration of 500 μg·mL−1. Considering both the activities, AE was selected for separation of bioactive molecule by deploying two purification techniques – column chromatography and preparative thin layer chromatography consecutively. After purification, the sample was injected into mass spectrometer and the presence of N-p-coumaroyltyramine and luteolin with excellent antibacterial and antioxidant properties (13.1 ± 2.2 mm and 80.9% ± 2.3%, respectively) were recognised. Further, in vivo investigations on Catla catla fingerlings infected with P. aeruginosa indicated that partially purified extracts cured the infection and resulted in a 100% survival rate.

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