UV spectrophotometric and HPLC methods have been developed and validated for the quantitative determination of remdesivir in pharmaceutical formulations. The HPLC analyzes have been performed on a C-18 column with a mobile phase consisting of 20 mM KH2PO4 solution and acetonitrile (50:50, v/v), at a flow rate of 1.2 mL min−1. UV spectrum has been recorded between 200 and 800 nm using deionized water as solvent and the wavelength of 247 nm has been selected. These methods have been validated according to the procedures described in ICH guidelines Q2(R1). Both methods demonstrated good linearity, precision and recovery. No spectral and chromatographic interferences from non-medicinal ingredients were found in both methods. Correlation coefficients were greater than 0.999 within a concentration range of 10–60 mg mL−1. Therefore both analytical methods gave the most reliable results for the quantification of remdesivir in pharmaceutical formulation.
It has become very important to offer species with high nutritional value as fresh or processed products for human consumption in their daily diet for balanced nutrition. In the scope of this study, 15 naturally grown European Cranberry bush (ECB) genotypes that naturally grown were characterized in terms of horticultural characteristics. Fruit length, fruit width, fruit weight, the number of fruits per each cluster and cluster weight were determined within the ranges of 8.78–10.96 mm, 7.93–10.84 mm, 0.21–0.70 g, 31–121, and 7.70–66.67 g, respectively. Ranking of the average values of examined organic acids obtained from all genotypes found as; malic acid (11,419 mg L−1) > citric acid (1926 mg L−1) > ascorbic acid (581 mg L−1) > oxalic acid (561 mg L−1). Total phenolic content (TPC) and total flavonoid content (TFC) were found at high levels in ECB with 2922–3475 mg gallic acid equivalent (GAE) L−1 and 1463–3163 mg quercetin equivalents (QE) L−1, respectively. While pomological characteristics were found to be highly positive correlated with each other, they were negatively correlated with chemical properties. Low pH was found to be an important parameter to obtain higher amounts of phytochemicals such as TPC, TFC, organic and phenolic acids correlated with strong antioxidant effects. The obtained results will be useful for both germplasm enrichment and cultivation.
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.
Cyclophosphamide (CP)—also known as cytophosphan—is an alkylating agent that has many side effects in humans and rats. Rats were divided into 5 different groups to evaluate the protective effect of escin (ES) obtained from the horse-chestnut plant (Aesculus hippocastanum) against acute damage induce by CP. Groups: control group, ethanol group, ES group (100 mg/kg body weight (bw) ES for 14 days by gastric gavage), ES + CP group (100 mg/kg bw ES for 14 days by gastric gavage and 75 mg/kg bw CP i.p. on 14th day), and CP group (75 mg/kg bw CP i.p. on 14th day). After the experiment was completed, blood and tissue samples (liver, kidney, heart, brain, lung, and testis) were taken from the rats under anesthesia. When the CP group was compared with the control group, an increase was observed in the level of Malondialdehyde (MDA) in blood and all tissues except the lung, but when it was given together with escin, there was a decrease except kidney and lung (P < 0.05). Glutathione (GSH) level decreased in the blood and all tissues when CP was given, whereas an increase was observed in the heart, brain, and lung when given with escin (P < 0.05). There was no statistical change in the activities of superoxide dismutase and catalase enzymes in all tissues. ES reduced CP-induced damage in all tissues except the kidney. As a result, it was determined that ES had a protective effect against CP-induced tissue damage in rats due to its antioxidant properties.
This study presents the development and validation of environmentally friendly analytical methods for quantifying Abiraterone Acetate (AA) in both its pure form and commercial pharmaceutical formulations. An optimized High-Performance Liquid Chromatography (HPLC) method was developed using an Agilent Extend C18 column (250 mm × 4.6 mm, 5 μm) at 25 °C. The mobile phase consisted of formic acid and ethanol in isocratic mode, with a flow rate of 1.0 mL min−1, and detection was performed at 253 nm. The spectrophotometric method involved a comprehensive evaluation of AA’s spectral properties in various solvents, with ultrapure water providing the most suitable spectra for analysis at 253 nm. Both methods were validated according to ICH guidelines, demonstrating selectivity, linearity, accuracy, precision, detection and quantification limits, and robustness, with correlation coefficients exceeding 0.999 across the 5–30 μg mL−1 concentration range. Comparative statistical analysis using Student’s t-test and Fisher’s F-test showed no significant differences between the two methods. The environmental impact of both methods was assessed using AGREE and GAPI software, confirming their sustainability. These validated methods offer reliable and eco-friendly approaches for the quantitative analysis of AA in tablet formulations, promoting safer and greener laboratory practices in pharmaceutical analysis.
Ibrutinib is a drug used for the treatment of marginal zone lymphoma, mantle cell lymphoma, lymphocytic leukemia, chronic graft, and Waldenstrom macroglobulinemia. A simple, sensitive, and fast liquid chromatographic and spectrophotometric method for the quantification of ibrutinib in pharmaceutical forms and bulk was developed and validated. The chromatographic technique was developed using an ODS 3 C 18 (250 mm × 4.6 mm i.d., 5 µm) column. The mobile phase was a mixture of 0.1% trifluoroacetic acid in water and acetonitrile (50/50, v/v) at a flow rate of 1.0 mL·min −1 . Eluent detection was carried out at a wavelength of 260 nm using a ultraviolet detector. The retention time of ibrutinib was found to be 5.27. On the other hand, Ibrutinib was determined using a spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 260 nm. The developed techniques were validated in accordance with the protocols outlined in International conference on harmonisation of technical requirements for registration of pharmaceuticals for human (ICH) guidelines Q2(R1). Correlation coefficients for both methods were greater than 0.999 in the concentration range of 5–30 mg·mL −1 . The relative standard deviation values were low in intraday and interday precision tests. The accuracy of the developed techniques ranged 99.74–100.23% for the chromatographic method and 99.32–100.76% for the spectrophotometric method. The limits of detection and quantitation were 0.90 and 2.80 µg·mL −1 for the chromatographic method and 1.10 and 3.20 µg·mL −1 for the spectrophotometric method. The developed and validated analytical methods can be safely used in quality control tests for the determination of the amount of ibrutinib in pharmaceutical products.