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Clobetasol Propionate is a highly strong corticosteroid that is used in a variety of topical medication formulations, including foam, ointment, lotion, spray and shampoo; with a dosage strength of 0.05% (w/w). The goal of this research was to identify and characterize a substantial unknown impurity (UK) detected during the stability testing of a Clobetasol Propionate foam pharmaceutical product in accelerated conditions (40°C and 75% relative humidity). Developing a single, robust and accurate HPLC method that is LC–MS compatible for quantifying all 14 potential Clobetasol Propionate impurities in therapeutic drugs is another goal. Preparative column chromatography was used to separate the impurity, and spectroscopic techniques like IR, NMR and MS were used to characterize its structure. The structure of isolated UK was effectively characterized and defined using spectroscopic data evaluation. The chromatographic method has also been validated according to the International Conference on Hominization's Q (2) quality guidelines. The isolated and characterized impurity had the same equivalence as the impurity found during stability testing. Precision, accuracy, linearity, robustness and ruggedness are all met in the method validation data. [ABSTRACT FROM AUTHOR]

Herein we demonstrated the preparation of sulphur-doped graphene (SG) prepared via hydrothermal route. The resulted material is used for making highly sensitive and selective electrochemical sensor platform for accurate quantification of Hydrogen Peroxide (H2O2). Structural features and surface morphology of synthesised materials are fully examined using High resolution Transmission electron microscopy (HRTEM), Scanning electron microscopy (SEM), FT-IR and Raman spectroscopy techniques. In addition to that, electrochemical techniques like cyclic voltammetry (CV) and chronoamperometry (CA) are used to quantify the electron transfer kinetics and electro catalytic activity, these results inveterate it is due to strong electron donating ability of doped sulphur (S) atom and edge plane sites in SG that promotes the electron transfer process at electrode-electrolyte interface. The SG modified glassy carbon electrode (SG/GCE) exhibited finite selectivity; sensitivity stability with a regression coefficient (R2) value is 0.99 towards H2O2 estimation. The above observation conclude that these results are finest report to scrutinise the electrochemical properties of Graphene network by doping with Sulphur atom and it served as an important benchmark for the development of inexpensive SG based sensor platforms for electrochemical biosensor applications. [ABSTRACT FROM AUTHOR]

Dasatinib is an aminopyrimidine used as an inhibitor of multiple tyrosine kinases in two different formulations an immediate-release tablet and a powder for oral suspension. It shows a very low pH-dependent solubility in aqueous solutions and higher solubility in organic solvents. The solubility plays an essential role in analytical methodology to establish the purity, potency, safety and efficacy of any drug product as a diluent. Also, extraction of active drug substance with a suitable diluent from matrix composition is crucial for any analytical method development. However, a diluent optimization study during the method development of related substances for the drug product reveals that the Piperazine ring presented in Dasatinib is susceptible to oxidation and forms an N-oxide impurity. The impurity formation is due to the micro oxidic properties of the solvent used as a diluent which is inducing an oxidation reaction. Therefore, a comprehensive investigative study was conducted to optimize the diluent by limiting N-Oxide generation. [ABSTRACT FROM AUTHOR]

The present work describes the synthesis of molnupiravir by employing commercially available inexpensive materials in two steps with an overall yield of 85.7%. The synthetic methodology starts with an eco-friendly starting material, that is, cytidine and establishes an alternative way to avoid costly enzyme mediated reactions. This synthetic strategy involves a selective acylation of cytidine as the first key step followed by the second step, that is, hydroxamination reaction. The major advantage of this protocol is that it is completely free of protection and deprotection reactions. Chemoselective acylation of cytidine's primary alcohol was achieved using isobutyryl chloride, Et3N, and DMF solvent (89.3% yield). The aqueous phase transformation was achieved for the hydroxamination reaction with a 96% yield. [ABSTRACT FROM AUTHOR]

Background: A kind of estrogen called estradiol is a female sex hormone that regulates several body processes. In hormone replacement therapy for women, the endogenous steroid progesterone is employed. The soft gel capsule medication, which contains a mix of 1 mg estradiol and 100 mg progesterone, is used to treat moderate to severe menopause symptoms, such as hot flashes, in women who have uteruses, as well as feelings of warmth in the face, neck, and chest. Objective: To establish the stability of drug products in accordance with the ICH Harmonized Tripartite Guideline, Stability Testing of New Drug Substances and Products (Q1A), this study aims to develop a reverse-phase chromatographic method, the necessary analytical methodology for identifying the drug degradation profiles. Method: The procedures were optimized using a C18 column (250 4.6 mm, 5 m) as the stationary phase and conventional solvents such as water–acetonitrile mixtures as the mobile phase. A quantification technique had been an HPLC combined with a UV/PDA and fluorescence detector. Results: The developed methods for both estradiol and progesterone were capable of all components of each active individually by overcoming the extremely difficult challenges of a combination product with similar structural compounds, having 24 impurities in all, and having complex excipients used for soft gel formulation. Conclusions: The method has been successfully created, validated for use in compliance with regulatory specifications, and determined to be accurate, linear, specific, and stability-indicating in nature. Highlights: To quantify the associated impurities of both actives in the presence of a highly complex matrix, the performance of the HPLC approach considerably possesses a higher degree of selectivity. [ABSTRACT FROM AUTHOR]

The medicinal plant Morinda tinctoria Roxb. is used in the treatment of various diseases traditionally. Report on bioactive evaluation of M. tinctoria Roxb. has led us to the phytochemical examination of M. tinctoria leaves. Our objective was to isolate compounds form M. tinctoria Roxb. and characterize each compound. The isolated compounds were tested for antioxidant, antimicrobial, antiobesity, cytotoxicity and genotoxicity properties. For this work, we have chosen solvents with increasing polarities. Hexane, chloroform, ethyl acetate and methanol were used in this study. The solvent extracts were analyzed using column chromatography and the isolated compounds were characterized using FTIR, ¹H NMR, 13C NMR and mass spectra. The constituents have been characterized and screened for in vitro antioxidant, antimicrobial, antiobesity, cytotoxicity and genotoxicity properties. Nine bioactive compounds were isolated and identified: palmitic acid, fucoxanthine, broussin, isoliquiritigenin, cynarin, gallic acid, β-sitosterol, quercetin and oleuropein. The results thus indicate conclusively that M. tinctoria leaves possess various potent bioactive compounds and is therefore recommended as a plant of phytopharmaceutical importance. [ABSTRACT FROM AUTHOR]

The antioxidant activity and total phenolic content of Morinda tinctoria leaves was evaluated. The successively extracted leaves of Morinda tinctoria using various solvents was analyzed for their total phenolic content. The extracts were subjected to column chromatography for the isolation of bioactive molecules. In vitro antioxidant activity was evaluated by employing different assays, including 2,2-diphenyl-1-picrylhydrazyl, nitric oxide scavenging assay and phosphomolybdenum reducing power assay. The 2,2-diphenyl-1-picrylhydrazyl radical scavenging efficacy of hexane extract is significant at higher concentration (500 µg/ml - 91.2 ± 0.05%) and the efficacy at lower concentration is more significant for ethyl acetate extract (100 µg/ml - 65.1 ± 0.05%). The total phenolic content was highest in methanol extract (5.30 ± 0.011 µg/mg). Cynarin, a hydroxy cinnamic acid was isolated from chloroform extract; oleuropein, a polyphenolic iridoid was isolated from methanol extract. The results obtained suggested that Morinda tinctoria leaf extracts possessed antioxidant properties and might offer protection from free radicals. Two compounds, cynarin and oleuropein were reported for the first time from Morinda tinctoria leaves. [ABSTRACT FROM AUTHOR]

Background: Rifaximin, a medication of the rifamycin family with two distinct strengths of 200 mg and 550 mg in tablet form, is useful for the treatment of travelers' diarrhea. It has a solid yellow hue and is very hygroscopic in nature. It exhibits a variety of polymorphic forms such as a, b, c, d, and e depending on bonded moisture. These polymorphs' varying chemical and physical characteristics, such as solubility and water content, may have a big impact on in vivo absorption, which in turn affects efficacy and safety. Therefore, understanding the polymorphic stability of rifaximin is crucial for formulating rifaximin tablets. Objective: The current effort focuses on the understanding of water vapor sorption properties to control the polymorphic stability of rifaximin in the tablet formulation using the appropriate selection of excipients and manufacturing process. Methods: The dynamic vapor sorption method in the range of 0-90% relative humidity at 25C is used for understanding the sorption properties of drug substances and drug excipient mixtures; the state-of-the-art techniques of the X-ray diffraction method are used to identify polymorph conversions; and dissolution procedures are used for in vitro correlation studies. Results: The sorption study data reveals that rifaximin is highly unstable at relative humidity conditions above 36%. When using excipients that have a low tendency to adsorb water in the formulation, the polymorphic results do not show any change in their intended form, and the in vitro dissolution data show an equivalency with the reference drug product. Conclusion: The study prompted a successful outcome-oriented development of the formulation processing environment conditions design to develop a test formulation that has adequate polymorphic stability and also similarity in in-vitro dissolution profiles, with the reference product with highest similarity. Highlights: The overall study described here is useful for swiftly gaining insight into the sorption characteristics of rifaximin, and it contributes to the widespread acceptance of rifaximin tablets as a treatment option. [ABSTRACT FROM AUTHOR]

Dasatinib is an aminopyrimidine used as an inhibitor of multiple tyrosine kinases in two different formulations an immediate-release tablet and a powder for oral suspension. It shows a very low pH-dependent solubility in aqueous solutions and higher solubility in organic solvents. The solubility plays an essential role in analytical methodology to establish the purity, potency, safety and efficacy of any drug product as a diluent. Also, extraction of active drug substance with a suitable diluent from matrix composition is crucial for any analytical method development. However, a diluent optimization study during the method development of related substances for the drug product reveals that the Piperazine ring presented in Dasatinib is susceptible to oxidation and forms an N-oxide impurity. The impurity formation is due to the micro oxidic properties of the solvent used as a diluent which is inducing an oxidation reaction. Therefore, a comprehensive investigative study was conducted to optimize the diluent by limiting N-Oxide generation., (© The Author(s) 2022. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.)