Search Results (134)

Background: Fixed-dose combinations have advanced in many therapeutic areas, including otorhinolaryngology, where hearing disorders are increasingly prevalent. Objectives: The present study focuses on developing and evaluating a new capsule combining nicergoline (NIC), piracetam (PIR), and hawthorn extract (HE) for the management of sensorineural hearing loss. Methods: The first phase methodology comprised preformulation studies (DSC, FTIR, and PXRD) to assess compatibility among active substances and excipients. Subsequently, four formulations were prepared and tested for flowability, dissolution behavior in acidic and neutral media, and stability under oxidative, thermal, and photolytic stress. Quantification of the active substances and flavonoids was performed using validated spectrophotometric and HPLC-UV methods. Results: Among the tested variants, the F1 formulation (4.5 mg NIC, 200 mg PIR, 50 mg HE, 2.5 mg magnesium stearate, 2.5 mg sodium starch glycolate, and 240.5 mg monohydrate lactose per capsule) displayed optimal technological properties, superior dissolution in acidic media, and was further selected for evaluation. The antioxidant activity of the formulation was confirmed through the 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay, Trolox Equivalent Antioxidant Capacity (TEAC), and iron chelation tests, and was primarily attributed to the flavonoid content of the HE. Acute toxicity tests in mice and rats indicated a high safety margin (LD₅₀ > 2500 mg/kg), while ototoxicity assessments showed no adverse effects on auditory function. Conclusions: The developed formulation displayed good stability, safety, and therapeutic potential, while the applied workflow could represent a model for the development of future fixed-dose combinations. Full article

Soil washing is an efficient method to remove polybrominated diphenyl ethers (PBDEs) from contaminated soils. The obtained solutions from soil-washing still contain PBDEs, requiring further treatment before disposal or reuse. Although photolysis is effective for PBDE degradation in solutions, the concurrent formation of toxic polybrominated dibenzofurans (PBDFs) may limit its practical application. In this study, 2,8-dibromodibenzofurans (2,8-BDF) formation rate and mechanisms during 2,4,4′-tribromodiphenyl ether (BDE-28) photolysis in various simulated soil-washing solutions was investigated. Results revealed significant effects of solubilizers on 2,8-BDF formation. The nonionic surfactants polysorbate (TW80), polyoxyethylene octylphenyl ether (TX series), and the cationic surfactant cetyltrimethylammonium bromide (CTAB) resulted in low 2,8-BDF formation rate (1–5%), while the β-cyclodextrin led to the highest 2,8-BDF formation rate (about 28%). The nonionic surfactants polyoxyethylene dodecyl ethers (Brij series), and the anionic surfactants sodium dodecylbenzene sulfonate (SDBS) and sodium dodecyl sulfate (SDS), also showed a high level of 2,8-BDF formation rate (7–17%). Solubilizer structure and its interaction with BDE-28 determined the 2,8-BDF formation. The role of the micelle microenvironment on 2,8-BDF formation was verified via an experiment and molecular dynamics simulation. The organic region of micelle exhibited high hydrogen donation ability, which inhibited 2,8-BDF formation. The results indicated distinct risks of PBDE photolysis in various soil-washing solutions, providing an important reference for solubilizer selection and the application of photolysis on the treatment of soil-washing solutions containing PBDEs. Full article

Industrial growth led to the expansion of existing environmental problems, where different kinds of pollutants can enter the environment by many known routes, particularly through wastewater. Among other contaminants, pharmaceuticals, such as diazepam, once released, pose a significant challenge related to their removal from complex environmental matrices due to their persistence and potential toxicity. For this reason, it is a great challenge to find suitable methods for the treatment of wastewater. The aim of this paper was to investigate the stability of diazepam, subjecting it to various degradation processes (hydrolysis and photolysis), focusing on photocatalysis, an advanced oxidation process commonly used for the purification of industrial wastewater. The photocatalytic system consisted of UV-A and simulated solar irradiation with titanium dioxide (TiO₂) immobilized on a glass mesh as a photocatalyst, with an additional reaction performed in the presence of an oxidizing agent, i.e., hydrogen peroxide, to improve diazepam removal from water matrices. The kinetic rate of diazepam degradation was monitored with a high-performance liquid chromatograph coupled with a photodiode array detector (HPLC-PDA). The target compound was characterized as a hydrolytically and photolytically stable compound with t_1/2 = 25 h. The presence of an immobilized TiO₂ catalyst contributed significantly to the degradation of diazepam under the influence of UV-A and simulated solar radiation, with t_1/2 in the range of 1.61–2.56 h. Five degradation products of diazepam were identified at the laboratory scale by MS analysis (m/z = 267, m/z = 273, m/z = 301, m/z = 271, and m/z = 303), while the toxicity assessment revealed that diazepam exhibited developmental toxicity and a low bioaccumulation factor. The pilot-scale process resulted in significant improvements in diazepam degradation with the fastest degradation kinetics (0.6888 h⁻¹). These results obtained at the pilot scale highlight the potential for industrial-scale implementation, offering a promising and innovative solution for pharmaceutical removal from wastewater. Full article

The conversion of biomass towards value-added and platform chemicals has become the focus of extensive research these past two decades. One of the methods that has been increasingly studied is the use of semiconductor-mediated photocatalysis for biomass conversion. Titanium dioxide has previously been demonstrated to be an effective commercial catalyst for the cleavage of bonds within lignin and also cellulose and hemicellulose. Described herein is the deployment of TiO₂ for the cleavage of bonds within two β-O-4 lignin model compounds, one bearing a ketone in the α-position and the other an alcohol. The presence of a ketone in the benzylic position in one of the models had a pronounced effect under photolytic conditions, e.g., in the absence of a photocatalyst but with irradiation present. The subsequent reduction of the benzylic ketone resulted in observed sensitivity towards the irradiation and solely photocatalytic conversion was achieved. In addition, reaction products are proposed, which demonstrate a feasible method for β-O-4 cleavage in native lignin extracts. Full article

An aqueous mixture of three compounds (atrazine, carbamazepine, and p-chlorobenzoic acid) has been treated by photochemical processes including photolysis and photocatalysis with 10.7% TiO₂ supported on ceramic foams of mullite. Experiments were conducted in both ultrapure water and in a secondary effluent from a municipal wastewater treatment plant. Radiation at 365 nm was totally inefficient in the photolytic process carried out in ultrapure water; however, some sensitization phenomena were observed when municipal wastewater was used as a bulk matrix. In the latter case, conversion values in the range of 20–30% were obtained after 2 h. The photocatalytic process was much more effective experiencing conversions above 80% after just 80 min of reaction. The nature of the matrix used exerted a significant influence. Use of municipal wastewater slowed down the process due to the scavenging character of the natural organic matter content. Test runs in the presence of carbonates and t-butyl alcohol suggested that radical carbonates play some role in contaminant abatement, and secondary radicals generated after the t-BuOH attack by HO^● radicals should also be considered in the reaction mechanism. A pseudo-empirical mechanism of reactions sustains the experimental result obtained, acceptably modeling the effects of a water matrix, scavenger addition, and radiation volumetric photon flux. Full article

The use of ultraviolet (UV) for water disinfection is known for its chemical-free process and with no harmful disinfection by-products. Yet, the disinfection process remains time-consuming, and many studies are limited to disinfection of one or two microbial species. Direct photolytic and glass-embedded TiO₂ photocatalytic disinfection of four different bacterial species (Staphylococcus aureus, Salmonella senftenberg, Bacillus subtilis, and Escherichia coli) were assessed using UV-LED radiation with wavelengths of 365 nm. The optimization of the UV disinfection under different masses of the TiO₂ photocatalyst was evaluated. Additionally, the order of disinfection of the different bacteria species was assessed. The disinfection effects were measured based on the potential to reduce the number of bacteria species, calculated in colony-forming units/mL and log reduction units. The disinfection of Staphylococcus aureus was enhanced from 1.46 log reduction units in the UV-alone treatment to a high of 5.65 log reduction units in the UV + 0.08 g TiO₂ treatment. Regarding Salmonella senftenberg, disinfection was enhanced from 1.26 log reduction units to 3.85 log reduction units in UV-alone experimental treatments and UV + 0.04 g TiO₂, respectively. Similarly, an increase in Bacillus subtilis reduction was achieved from a low of 0.69 log reduction units to a high of 2.98 log reduction units in UV-alone treatments and UV + 0.08 g TiO₂, respectively. The disinfection of Escherichia coli was enhanced from 2.49 log reduction units (UV-alone treatment) to a high of 6.35 log reduction units (UV + 0.02 g TiO₂). The findings provide key implications and new insights into the studied bacteria species and the future application of porous glass-embedded TiO₂ photocatalysts to enhance bacteria disinfection using UV light for improved water. Full article

An isocratic reverse-phase high-performance liquid chromatography (RP-HPLC) method, coupled with photodiode array detection (PDA), was developed for the identification and characterization of stress degradation products and an unknown process-related impurity of rivaroxaban in bulk drug form. Rivaroxaban, a selective and direct Factor Xa inhibitor, underwent forced degradation under hydrolytic (acidic, alkaline, and neutral), photolytic, thermal, and oxidative stress conditions, following the ICH’s guidelines. The drug displayed significant susceptibility to acid, base, and oxidative environments leading to the formation of eleven degradation products. All degradation products, along with process impurities and Rivaroxaban, were effectively separated using a (4.6 × 250 mm, 5 µm) C18 Thermo ODS Hypersil column at ambient temperature. The mobile phase composed of acetonitrile and monobasic potassium phosphate (pH 2.9) in a 30:70 (v/v) ratio, with a flow rate of 1.0 mL/min, and detection was carried out at 249 nm. The LC-PDA method was validated in accordance with the ICH’s guidelines and USP38-NF33, demonstrating specificity, linearity, accuracy, precision, and robustness. Recovery studies showed results within the range of 98.6–103.4%, with a % RSD LT 2%. The limits of detection (LOD) and quantitation (LOQ) for rivaroxaban were determined to be 0.30 ppm and 1.0 ppm, respectively. Stress studies confirmed that the degradation products did not interfere with rivaroxaban detection, establishing the method as stability-indicating. Specific impurities were identified, including impurity G at 2.79 min, impurity D at 3.50 min, impurity H at 5.32 min, impurity C at 6.14 min, impurity E at 8.36 min, impurity A at 9.03 min, and impurity F at 9.49 min. Additionally, several unknown impurities were observed at 3.20, 4.00, 4.59, and 4.77 min. Statistical evaluation confirmed the method’s reliability, making it suitable for routine analysis, quality control of raw materials, formulations of varying strengths, dissolution studies, and bioequivalence assessments of rivaroxaban formulations. Full article

Photolabile protecting groups (PPGs), also known as caging groups, are valuable tools in photopharmacology. They enable precise control over the release of bioactive compounds from the corresponding caged compounds at a precisely controlled time and place using light of specific wavelengths. This study introduces a novel approach to fine-tuning the photophysical and photochemical properties of visible-light-sensitive dicyanocoumarin- and COUPY-based caging groups by incorporating a phenyl group in a position adjacent to the photolabile bond. Our photoactivation studies with visible light demonstrated that this structural modification slightly improved the photolytic efficiency of both dicyanocoumarin- and COUPY-caged model compounds compared to their methyl-substituted or unsubstituted counterparts. Furthermore, COUPY PPGs were efficiently photoactivated with red light (620 nm) and successfully used to cage two antitumor drugs, chlorambucil and 4-phenylbutyric acid. These findings highlight the potential of phenyl-containing caging groups based on dicyanocoumarin and COUPY scaffolds as versatile platforms for developing new light-activated tools for photopharmacology applications. Full article

Natural pigments like betacyanins are highly unstable under heat, light, acid, and alkaline conditions. Yeast protein (YP) is a promising substitute protein, while chitooligosaccharides (COS) are water-soluble alkaline polysaccharides. Water-in-oil-in-water (W₁/O/W₂) emulsions, with two-membrane, three-phase structure, can serve as effective carriers for stabilizing pigments. In this study, YP-COS complexes formed through electrostatic interactions were used as hydrophilic emulsifiers to create betacyanin-coated W₁/O/W₂ emulsions. The W₁/O colostrum was designed to make up 30%, 70%, and 90% of the emulsion (v/v)and the W₂ was designed by the complexes with three concentrations of YP (2%, 1.25% and 0.5%, w/v)-COS (6%, 3.75% and 1.5%, w/v). The optimal formulation was determined through comprehensive evaluation of micromorphological characteristics, particle size, zeta potential and creaming index, ultimately yielding a system comprising YP (2%)-COS (6%) and 90% W₁/O colostrum. Moreover, the W₁/O/W₂ emulsion system significantly improved the betacyanins retention under thermal treatment, photolytic exposure, pH gradients, and extended storage compared to the betacyanin aqueous solution (p < 0.05). In vitro digestion tests showed the emulsion retained 58.39% of betacyanins, while the betacyanin aqueous solution retained only 41.42%, demonstrating the emulsion’s ability to delay the betacyanins release, offering new insights for using YP-COS complexes in food production and other fields. Full article

In this study, we thoroughly investigated the stability of haloperidol using a comprehensive set of chromatographic and thermal analyses. Various stress conditions were examined, including exposure to oxidizing agents (such as hydrogen peroxide), dry heat, photolytic conditions, and acid and alkaline hydrolysis. Significant degradation was observed in acidic and alkaline environments, leading to the formation of degradation by-products, specifically DPA, DPB, DPC, and DPD for acidic and basic conditions. In contrast, haloperidol demonstrated robust stability under photolytic, oxidative, and dry-heat conditions. For the analysis of the drug and its degradation products, a C-18 column was employed, coupled with a mobile phase consisting of methanol and a phosphate buffer (pH = 9.8) in a 90:10 (v/v) ratio. The analytical method was rigorously validated according to ICH Q2 (R1) guidelines, ensuring its accuracy and reliability. This method exhibited excellent linearity within a concentration range of 1 to 50 µg/mL, with an R² of 0.999. Additionally, this method is applicable to commercial formulations, without the need for prior extraction. LC-MS/MS analysis revealed distinct m/z values and fragmentation spectra corresponding to the degradation products, including an impurity not documented in the European Pharmacopoeia monograph for the drug. Three additional degradation products were identified based on m/z values and base fragments. Thermal analyses, including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and differential thermal analysis (DTA), provided further evidence of the active ingredient’s thermal stability, with a melting temperature of approximately 150 °C. These results collectively offer valuable insights into the degradation behavior of haloperidol, providing critical implications for its pharmaceutical quality and integrity under various environmental conditions. Full article

Textile dyes pose a major environmental threat due to their toxicity, persistence in water bodies, and resistance to conventional wastewater treatment. To address this, researchers have explored biological and physicochemical degradation methods, focusing on microbial, photolytic, and nanoparticle-mediated approaches, among others. Microbial degradation depends on fungi, bacteria, yeasts, and algae, utilizing enzymatic pathways involving oxidoreductases like laccases, peroxidases, and azoreductases to breakdown or modify complex dye molecules. Photolytic degradation employs hydroxyl radical generation and electron-hole pair formation, while nanoparticle-mediated degradation utilizes titanium dioxide (TiO₂), zinc oxide (ZnO), and silver (Ag) nanoparticles to enhance dye removal. To improve efficiency, microbial consortia have been developed to enhance decolorization and mineralization, offering a cost-effective and eco-friendly alternative to physicochemical methods. Photocatalytic degradation, particularly using TiO₂, harnesses light energy for dye breakdown. Research advancements focus on shifting TiO₂ activation from UV to visible light through doping and composite materials, while optimizing surface area and mesoporosity for better adsorption. Nanoparticle-mediated approaches benefit from a high surface area and rapid adsorption, with ongoing improvements in synthesis, functionalization, and reusability, particularly through magnetic nanoparticle integration. These emerging technologies provide sustainable solutions for dye degradation. The primary aim of this review is to comprehensively evaluate and synthesize current research and advancements in the degradation of azo dyes through microbial methods, photolytic processes, and nanotechnology-based approaches. The review also provides detailed information on salient mechanistic aspects of these methods, efficiencies, advantages, challenges, and potential applications in industrial and environmental contexts. Full article

Background/Objectives: Janus kinase inhibitors open new horizons for small-molecule drugs in treating inflammatory bowel disease, with ritlecitinib demonstrating significant efficacy in clinical trials for ulcerative colitis and Crohn’s disease. Ritlecitinib, a second-generation JAK3 inhibitor, is a novel therapeutic agent for alopecia areata and other autoimmune conditions. Methods: A new stability-indicating UHPLC-DAD-MS/MS method was developed, validated, and applied for a forced degradation study of ritlecitinib under ICH guidelines. Results: The method demonstrated high specificity, sensitivity (LOD: 0.04 µg/mL; LOQ: 0.14 µg/mL), precision (RSD ≤ 0.15%), and accuracy (99.9–100.3%). Forced degradation studies under acidic, basic, oxidative, thermal, and photolytic conditions revealed four novel degradation products. Basic degradation followed second-order kinetics, while oxidative degradation followed zero-order kinetics. Conclusions: The validated method reliably characterized ritlecitinib’s stability and degradation products, providing essential data for optimizing formulation, determining proper storage conditions, anticipating drug–excipient interactions, and ensuring quality control. The eco-friendliness and applicability of the developed forced degradation procedure were evaluated using various green and blue metric tools. Incorporating green analytical principles underscores its potential for sustainable pharmaceutical analysis. Full article

Hydroperoxymethyl thioformate (or HPMTF) is a compound relevant to the chemistry of sulfur in the marine atmosphere. The chemical cycling of this molecule in the atmosphere is still uncertain due in part to the lack of accurate knowledge of its photolytic behavior. Only approximations based on the properties of its chromophores are used in previous studies. In this work, we calculated the absorption spectra of the molecule in gas and aqueous phases using the Nuclear Ensemble Approach (NEA) and the CASPT2 method. Furthermore, we used such information to obtain relative photolysis rates. We found that the chromophore approximation overestimates the photolysis rates in the gas phase by twice the value obtained with the NEA-CASPT2 protocol. Furthermore, for the aqueous phase, we predict a lower role of photolysis as compared to the gas phase. Full article

Ginsenoside Re was the major bioactive component found rich in Panax ginseng C. A. Meyer, which exerted excellent cardiovascular protection, anti-inflammatory, and anti-oxidation effects. The generation of unexpected degradation products (DPs) may influence the therapeutic effect of Re, or even bring toxic effects to patients. However, to date, only a few reports were available about the stability of Re. The present study aims to systematically investigate the degradation behaviors of Re under different stress conditions, including hydrolysis (acidic, basic, and neutral), oxidation, humidity, thermal, and photolytic (ultraviolet and visible light) conditions. A total of thirteen DPs were putatively identified, and among them, nine were discovered for the first time in our study. The results showed that Re was sensitive to exposure to acidic, basic, and oxidation conditions. It underwent a series of chemical degradation reactions, including deglycosylation, dehydration, addition, oxidation at the double bond, and isomerization under various stress conditions. Structural characterization of these DPs was carried out by UHPLC-DAD-CAD and LC-LTQ/Orbitrap. A plausible mechanism of their formation was proposed to support the structures of all DPs of Re. In silico toxicity prediction and metabolism behavior assessment were done by Derek Nexus and Meteor Nexus software. Re and DP-1 to DP-6 were predicted to possess potential skin irritation/corrosion toxicity. DP-11 and DP-12 bear the potential for carcinogenicity, mutagenicity, irritation, hepatotoxicity, and skin sensitization. The observation of these DPs updates our knowledge regarding the stability of Re, which provides valuable information for quality control and to choose suitable storage conditions. Full article

Nano metal oxides (NMOs), with their unique physico-chemical properties and low toxicity, have become a focus of research in heterogeneous catalysis. Their distinct characteristics, which can be tailored based on size and structure, make them highly efficient catalysts. NMOs have the potential to significantly contribute to the degradation of numerous environmental pollutants through photolytic decomposition. This work comprehensively analyzes the synthesis, catalytic performance, and applications of photocatalytically active metal oxides, specifically titanium, zinc, copper, iron, silver, tin, and tungsten oxides. The primary objective is to demonstrate how the effectiveness of photocatalytic processes can be enhanced and optimized by incorporating metals, non-metals, and metalloids into their structure and forming heterostructures. Furthermore, the aim is to understand the underlying process of photocatalytic oxidation thoroughly. Photocatalysis, a promising approach in advanced oxidation processes, has garnered significant interest in these fields. Full article