Band 45, Heft 1

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.

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.

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.

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.