Abstract This work develops and validates a green reverse-phase “high-performance thin-layer chromatography (HPTLC)” methodology for measuring fenofibrate (FEN) and rosuvastatin (ROS) concurrently in commercially available fixed-dose combination (FDC) tablets. A green developing system comprising ethanol, water, and ammonia solution (25 % for HPLC) in a 65:30:5 (v/v/v) ternary ratio was used to analyze FEN and ROS concurrently. At a wavelength of 265 nm, FEN and ROS were both concurrently measured. The method’s greenness profile was evaluated using three different greenness methodologies: the analytical eco-scale (AES), chloroform toxicity (ChlorTox), and the analytical GREEnness (AGREE). The developed method was linear for both drugs in the 20–1,200 ng/band range. The developed method was validated and shown to be reliable, sensitive, accurate, precise, and eco-friendly. The results of every greenness tool, such as AES (87), ChlorTox (0.78 g), and AGREE (0.78) demonstrated that the proposed method had an exceptionally greenness profile. The levels of FEN and ROS in two different marketed FDC products were found to be within the 100 ± 2 % limit using the current methodology. The study’s findings demonstrated that the suggested technique could reliably evaluate FEN and ROS in commercially available products.

Abstract This study aims to develop and experimentally implement a novel portable electrochemical sensor based on screen-printed carbon electrodes (SPCEs) and an original bath-injection electrochemical cell for real-time environmental monitoring of pollutants. The scientific novelty of this work lies in the design of a simplified yet highly effective electrochemical cell that eliminates the need for a liquid carrier through an innovative self-washing mechanism using excess sample volume. This feature significantly reduces system complexity and enhances sensor reliability in field applications. The advantages of microfluidic technologies in the development of SPCE-based sensors are highlighted, and detailed protocols for modifying SPCEs with mercury, bismuth, and gold films are presented. Surface characterization is supported by micrographs, ensuring reproducibility of the electrode surface and analytical results. Voltammograms for various individual ions and their mixtures are provided, along with the corresponding electrode modifications and analytical conditions. The developed system demonstrates a broad linear concentration range and a detection limit as low as 5–10 μg/L. Field trials of the sensor were conducted using water samples from the Zeravshan river, a major source of drinking water in the region. Elevated concentrations of several toxic ions were detected, with the results confirmed by atomic absorption and inductively coupled plasma atomic emission spectroscopy. The proposed sensor system proves to be a promising solution for on-site pollutant detection under limited infrastructure conditions, supporting rapid response to both anthropogenic and natural environmental emergencies.

Abstract Selective androgen receptor modulators (SARMs), including andarine (S-4), have gained significant attention in the dietary supplement market despite their known health risks and prohibition in competitive sports. Although andarine remains widely available, data on its actual presence in dietary supplements are limited. To address this gap, this study assessed the quality of dietary supplements marketed as containing andarine. An HPLC–HRMS method was developed, validated, and applied to analyze three commercially available dietary supplements. HRMS (QTOF) detection, in MS as well as MS/MS regimes, was essential for confirming the presence of andarine and unexpectedly identifying other biologically active substances, specifically the metabolic modulators SR9009 and GW501516, based on precise molecular weights of precursor and product ions relative to reference standards. The analysis revealed discrepancies between the labeled and actual contents of the analyzed dietary supplements. These findings underscore the potential health risks posed by mislabeled and adulterated dietary supplements and highlight the urgent need for stricter quality control and regulatory oversight in the dietary supplement industry.

Abstract Shilajit (Mumijo) is a phytomineral exudate known for its therapeutic potential, traditionally used in Ayurvedic medicine. Its molecular composition and consequently its therapeutic properties are influenced by geographical origin. Low-field nuclear magnetic resonance (LF NMR) offers a non-destructive tool to assess the molecular behavior of Shilajit rapidly and non-destructively. Twelve raw Shilajit samples from five regions (Iran, India, Nepal, Russia, and Kyrgyzstan) were analyzed using LF NMR at 15 MHz. Longitudinal magnetization relaxation ( T 1 ) and transverse magnetization relaxation ( T 2 ) relaxation times were measured using an inversion-recovery and Carr–Purcell–Meiboom–Gill pulse sequence, respectively. Three distinct relaxation behavior groups were identified. Group I showed only T 1 (solid samples with undetectable T 2 ), group II exhibited single T 1 and T 2 (moderately viscous, hydrated samples), while group III revealed biphasic T 2 relaxation (indicating proton heterogeneity). Clear differences in relaxation profiles were observed across geographical origins, with Iranian samples showing the widest range of T 1 values, while Russian and some Iranian samples exhibited dual T 2 components. LF NMR relaxation parameters ( T 1 , T 2 ) are strongly dependent on the geographic origin and molecular structure of Shilajit. The technique shows promise for use in authentication and traceability of Shilajit, enabling differentiation based on relaxation signatures.

Abstract The study presents the development of a novel, sustainable, and analytical quality by design (AQbD) driven RP-HPLC method to simultaneously identify disodium edetate in eye drops and its degradation products. The goal of this method is to meet the growing demand for robust, eco-friendly methods of quality control for pharmaceutical products. AQbD ensured method robustness, while minimizing solvent consumption and waste generation to ensure sustainability. Several sustainable tools were investigated to assess their ecological impact in the study. Using Box–Behnken design, three chromatographic parameters were optimized: column oven temperature, flow rate, and buffer pH. An ethanol and tetrabutylammonium hydroxide solution mobile phase at pH 7.0 in gradient mode was found to be optimal. An Avantor Hichrom C18 (4.6 mm × 150 mm, 5 µm) column was used with UV detection at 258 nm and pumped at 1.1 mL/min. The linearity of disodium edetate occurred in the 2–40 μg/mL range with an R 2 of 0.9999. Disodium edetate was subjected to acidic, basic, oxidative, photolytic, and thermal stress conditions in accordance with ICH guidelines. Degradation caused by bases, acids, and oxidation provided the highest degradation rates. Incorporating quality by design principles with sustainability considerations makes this method robust, eco-friendly, and cost-effective for quality control in pharmaceutical products. Having been successfully applied to eye drop formulations, its utility in the pharmaceutical industry is unquestionable.

Abstract Deuterium is a heavy nonradioactive isotope of hydrogen, present in ocean water at a concentration of around 150 parts per million (ppm). In terrestrial nature, deuterium content in water varies by at least a factor of two, while in industry and research, the whole range of deuterium concentrations is employed. Water with altered deuterium content is currently of increasing interest in biology and medicine. Therefore, accurate measurements of deuterium content in water are an important problem. Historically, such measurements have relied on densitometry and mass spectrometry. More recently, alternative techniques emerged, such as Fourier Transform Infrared (FTIR) spectroscopy, varieties of Laser Spectroscopy (LS), Off-Axis Integrated-Cavity Laser Spectroscopy (OA-ICOS), nuclear magnetic resonance (NMR) spectroscopy, original research developments based on two-dimensional diffuse laser scattering (2D-DLS), and isotopic fractionation in metalloorganic nanotubes (MONTs). This review aims to provide brief description of the techniques currently in use for measuring deuterium content in water, evaluate their analytical performance and applicability across different contexts, and discuss the broader implications of these measurements in scientific research.

Abstract The sustainability and effectiveness of the chemical industry are greatly enhanced by white and green chemistry. Ten sustainability tools have been developed based on green and white metrics. Several tools can be used to determine how environmentally friendly, innovative, and forthright reversed-phase ultra-performance liquid chromatography (RP-UPLC) and ultraviolet (UV) techniques can simultaneously analyze and separate metformin (MET) and dapagliflozin (DAP) in pure and dosage forms. In addition to the green analytical procedure index and complex green analytical procedure index, analytical greenness, analytical greenness metric for sample preparation, eco-scale assessment, analytical method greenness score, high-performance liquid chromatography-environmental assessment tool, analytical method volume intensity, RGB12, and blue applicability grade index, several tools can be used to evaluate the effectiveness of these techniques. In the RP-UPLC methods under investigation, the isocratic technique was used to configure the optimal system. For RP-UPLC processes, a Waters XSelect HSS T3 C18 column (10 cm × 0.21 cm, 5 μm) was utilized. The sample and column oven temperatures were adjusted to 5°C and 35°C, respectively. The mobile phase in an RP-UPLC procedure was phosphate buffer and ethanol (55:45, v/v) adjusted to pH 7.0 with a 2 min duration, 2.0 μL injection volume, 0.5 mL·min −1 flow rate, and 225 nm UV detection. The second technique was the mean centering of ratio spectra (MCR) method, efficiently resolving the medications’ spectral overlapping at 257.7 and 240.9 nm for MET and DAP, respectively. For every drug, the correlation coefficient between the calibration curves for the UPLC and MCR techniques was more significant than 0.999. With primary recovery rates varying from 99.5% to 100.9%, the strategy produced good results. A validation process has been initiated pursuant to the principles of the International Council for Harmonisation.

Abstract An electrochemical sensor for cinchocaine (CIN) detection was developed based on surface molecular imprinting technology utilizing screen-printed gold electrodes modified with TiO 2 nanoparticles and electropolymerized polypyrrole. A novel sensor was developed using a dual-stage methodology, which entailed initial CIN template immobilization and subsequent electrochemical pyrrole polymerization incorporating titanium dioxide nanoscale particles. The sensor exhibited enhanced electroactive surface area (0.075 cm 2 ) and improved electron transfer kinetics (heterogeneous rate constant 8.2 × 10 −3 cm·s −1 ) compared to unmodified electrodes. Under optimized conditions (pH 5.0, 15-min incubation), the sensor demonstrated two linear response ranges from 0.1–10 and 10–100 μM, with a detection limit of 0.035 μM. The sensor showed excellent selectivity against common interferents, including a 100-fold excess of inorganic ions and a 50-fold excess of structurally similar compounds. Analysis of clinical samples yielded excellent recoveries (97.2–102.3%) with relative standard deviations below 4.3%. The simple fabrication process, rapid response time, and minimal sample preparation requirements make this sensor particularly suitable for point-of-care applications.

Abstract An innovative green reverse phase high-performance liquid chromatography method was developed and validated for the concurrent quantification of methocarbamol (MTC) and etoricoxib (ETC) in rat plasma using diclofenac potassium as an internal standard. This method introduces significant advancements over existing chromatographic techniques, including a rapid analysis time (8-min run time) and cost efficiency due to low solvent consumption (total solvent use of 444 mL), achieved through optimized chromatographic conditions. The method employs a Hypersil BDS C8 column (4.6 mm × 250 mm, 5 µm) with an isocratic mobile phase (buffer pH 2.5:methanol, 34:66 v/v) at 1.5 mL·min −1 and 274 nm detection. Linearity (1–50 µg·mL −1 , R 2 > 0.999) was demonstrated with sensitive detection limits (LOD = 0.20 µg·mL −1 [MTC], 0.25 µg·mL −1 [ETC] and LOQ = 0.60 µg·mL −1 [MTC], 0.75 µg·mL −1 [ETC]). Environmental sustainability was rigorously confirmed using eight green metrics (AGREE, ComplexGAPI, AMVI), yielding an analytical eco-scale score of 84, surpassing conventional methods in eco-friendliness . In vivo studies on complete Freund’s adjuvant-induced rheumatoid arthritis rats revealed the MTC–ETC combination’s potent anti-inflammatory and anti-arthritic effects, including reduced serum c-reactive protein levels ( p < 0.05) and preserved hepatorenal function. Validated per United States Food and Drug Administration guidelines, this method offers a fast, economical, and eco-conscious solution for pharmacokinetic studies and therapeutic monitoring, positioning the MTC–ETC combination as a promising, safe therapy for rheumatoid arthritis.

Abstract Lead-cooled fast reactors (LFR), such as the ALFRED Demonstrator, are pivotal in advancing nuclear technology. This study presents a method for quantifying trace-level impurities generated through various nuclear reactions in lead coolant. It combines inductively coupled plasma mass spectrometry with Sr-resin-based matrix separation to analyze trace impurities in lead matrices. The Sr-resin effectively removes lead, a highly interfering matrix, enhancing the precision and reliability of detecting trace elements. The study evaluates the effectiveness of lead matrix removal and assesses the method’s reliability for monitoring trace impurities in LFR systems. The results indicate the method’s suitability for tracking small changes in lead composition during the operation of lead-cooled facilities.