Search Results (159)

The Stability Toolkit for the Appraisal of Bio/Pharmaceuticals’ Level of Endurance (STABLE) is introduced and proposed as a comprehensive tool and software to evaluate the stability of active pharmaceutical ingredients (APIs) under various stress conditions. In the pharmaceutical industry, stability testing is a critical step in the drug development process, ensuring the quality, safety, and efficacy of APIs. Traditional stability tests—such as real-time, accelerated, and forced degradation testing—often face challenges, including inconsistent interpretation and implementation across different regions and organizations. STABLE addresses these challenges by providing a standardized and holistic approach to assessing drug stability across five key stress conditions: oxidative, thermal, acid-catalyzed hydrolysis, base-catalyzed hydrolysis, and photostability. Beyond its role as an evaluation tool, STABLE also serves as a practical guide for chemists, encouraging a more complete and thoughtful approach to stability studies. While many investigations focus solely on acid- and base-catalyzed hydrolysis, other critical conditions—such as photostability—are often underexplored or entirely omitted. By highlighting the importance of evaluating all relevant degradation pathways, STABLE promotes more robust and informed stability testing protocols. The index utilizes a color-coded scoring system to quantify and compare stability, facilitating consistent assessments across different APIs. This paper discusses the methodology of STABLE, including the scoring system and specific criteria applied under each condition. This tool is introduced to reflect intrinsic degradation susceptibility under forced conditions. The software is freely available as an open-source tool at bit.ly/STABLE2025, enabling broader accessibility and implementation across the pharmaceutical research community. Full article

The dichromate ion (Cr₂O₇²⁻), a highly toxic chromium VI species, is widely used in industrial processes, generating serious environmental problems when released into water bodies. This investigation proposes the use of a functionalized polymer as an adsorbent material for its removal in the aqueous phase. Poly(butyl methacrylate) (PBMA) was synthesized and modified by impregnation with resorcinarenes derived from long-chain aliphatic aldehydes. To improve the affinity for the dichromate, the resorcinarenes were functionalized with sulfomethyl groups by treatment with Na₂SO₃. The resulting matrices were characterized using IR-ATR, ¹H-NMR, and ¹³C-NMR, and their adsorbent performance was evaluated via UV-Vis spectroscopy in batch extraction assays. The results showed that the functionalized polymer exhibited a higher adsorption capacity than the base polymer, reaching up to 81.1% removal at pH 5.0 in one hour. These results highlight the potential of PBMA as an effective support and raise a promising research perspective for functionalized resorcinarenes in the development of new materials for the treatment of contaminated water. Full article

The application of high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) in the analysis of peptide therapeutics demonstrates its capacity to achieve high sensitivity and selectivity, which are essential qualities for the expanding peptide therapeutic industry. Given the challenges posed by hydrophilic peptides in reversed-phase chromatography, we investigated the necessity of a derivatization procedure to improve chromatographic separation and quasimolecular ion fragmentation during MS/MS detection. We investigated how eight different derivatizing agents react with a hydrophilic lysine- and arginine-containing human ezrin peptide-1 (HEP-1) to identify the most suitable one. The results showed that the reaction of HEP-1 with propionic anhydride proceeds most rapidly and completely, providing a high and reproducible yield of the product, which has sufficient retention on the RP column. The 4-propionylated derivative of HEP-1, compared to the other derivatives considered, demonstrates the most pronounced MS/MS fragmentation. The retention time of 2.42 min allows the separation of the substance from the interfering components of the blood plasma matrix and provides a limit of quantification of 5.00 ng/mL, which allows the use of this derivatizing agent for subsequent applications in pharmacokinetic studies, and this approach can improve the analytical parameters of similar peptides in other HPLC-MS/MS studies. Full article

This study focuses on the stabilization of a natural hair dye derived from Lawsonia inermis L. (henna) and Indigofera suffruticosa (indigo). Although various formulations already exist, they are designed for immediate use and cannot be stored. Lawsonia, a primary component of the dye, tends to degrade after release. To ensure its stability, freeze-drying was implemented as a protective measure. Colorimetric analysis confirmed the dye’s ability to maintain an intense, uniform coloration even after multiple washing cycles. Stability tests demonstrate that freeze-drying effectively enhances the dye’s stability and capacity to retain its physical properties and color under various environmental conditions, demonstrating its potential for long-term use. The dye’s pH (5.05) aligns with the natural pH of hair, promoting cuticle sealing and improving hair health. Cytotoxicity tests confirmed the dye’s safety, showing no harmful effects. Gray hair exhibited a total color difference (ΔE) of 64.06 after the initial application, using natural gray hair as a reference. By the third application, ΔE increased to 69.86 and gradually decreased to 68.20 after 15 washing cycles, highlighting its long-term durability. Gray hair exposed to 720 h of UV radiation showed a ΔE of 17.34, whereas dyed gray hair exhibited a ΔE of 2.96 compared to non-UV-exposed samples. This indicates superior resistance to color degradation in dyed hair. Also, SEM imaging revealed the dye’s restorative effects, progressively improving hair cuticle structure with each application. Full article

Edible mushrooms are macroscopic fungi that have been recognized as the “new superfoods” due to their high nutritional and medicinal values. The aim of this study was to develop and optimize a method for the wet digestion of edible mushrooms using a closed digestion block for the determination of macro- and micronutrients (Ca, Cr, Cu, Fe, K, Mg, Mn, Ni, and Zn) using microwave-induced plasma emission spectrometry (MIP OES). For the digestion of the samples, a 2³ factorial design was used to evaluate the amount of HNO₃ 65% (m m⁻¹), H₂O₂ 30% (m m⁻¹) and the digestion time, in 500 mg of the sample (dry and crushed) at 200° C. The method was applied to eleven species of edible or medicinal mushrooms (edible cultivated from wild strains, wild edible, and commercials medicinal). The average concentrations (in mg kg⁻¹) showed higher levels of K (1442.85–17,534.97), Mg (1295.40–13,550.72), Fe (11.33–27.38), Zn (28.86–36.09), and Mn (10.22–10.97). This study contributed to the determination of the multi-element composition and nutritional potential of edible mushrooms from Brazil. Full article

This study investigated the spatial distribution and radiological risks of naturally occurring radionuclides (²²⁶Ra, ²³²Th, ⁴⁰K) in 37 soil samples from Zacatecas, located in north-central Mexico, using high-resolution gamma spectrometry. Results revealed ⁴⁰K concentrations (mean: 736.81 Bq kg⁻¹), nearly double the global average, while ²²⁶Ra (29.96 Bq kg⁻¹) and ²³²Th (29.72 Bq kg⁻¹) aligned with worldwide norms. Geoaccumulation indices identified moderate ⁴⁰K accumulation at 22 sites, with El Capulín classified as moderately contaminated (I_geo = 1.07). Radiological risk indices showed absorbed dose rates (62.52 nGy h⁻¹) and excess lifetime cancer risk (0.330 × 10⁻³) exceeding global thresholds by 4% and 14%, respectively. Multivariate analyses demonstrated strong Spearman correlations (ρ = 0.75–1.00) among risk indices, while spatial interpolation identified southern/western regions as high-risk zones. These findings emphasize the necessity of integrating spatial analysis with multivariate statistical techniques in environmental radioprotection frameworks. While most of the study area complies with international safety standards, the identified zones exceeding dose thresholds warrant prioritized management to mitigate potential cumulative health risks. Full article

A solid phase microextraction (SPME) method coupled with liquid chromatography (LC) and fluorescence/ultraviolet-diode array detection was developed for the simultaneous determination of quercetin and trans-resveratrol. The chromatographic, detection, and SPME extraction/desorption conditions were systematically optimized. The performance of four commercial SPME fibers—polyacrylate (PA), polyethylene glycol (PEG), polydimethylsiloxane (PDMS), and polydimethylsiloxane-divinylbenzene (PDMS-DVB)—was evaluated and compared with a homemade polydopamine (PDA)-coated fiber. While all of the fibers successfully extracted the target analytes, their efficiencies varied significantly. The PA, PEG, and PDA fibers demonstrated superior performance, exhibiting wide linearity ranges (0.03–1 µg/mL (PA and PEG) and 0.06–1 µg/mL (PDA) for quercetin, 0.01–1 µg/mL for trans-resveratrol); high sensitivity (LODs of 0.01 µg/mL (PA and PEG) and 0.02 µg/mL (PDA) for quercetin, 0.003 µg/mL for trans-resveratrol); and excellent precision. Among these, the polyacrylate coating delivered the best analytical performance and was selected for further application. The optimized method was applied to analyze winemaking by-products (seeds, skins, and stalks) using SPME on ethanol-macerated extracts subjected to brief ultrasonication. Quercetin and trans-resveratrol were quantified in pomace extracts at concentrations of 104.3 ± 8.2 µg/g and 38.5 ± 4.1 µg/g, respectively. Recovery experiments confirmed the method’s accuracy, with recoveries of 99.1 ± 7.4% for quercetin and 98.5 ± 9.8% for trans-resveratrol. This study establishes a reliable, sensitive, and efficient approach for the determination of these bioactive compounds in complex matrices, with potential applications in the food and pharmaceutical industries. Full article

Early detection of cancer can dramatically improve long-term prognosis and survivability in a variety of different cancer types. However, for many cancer types, the ability to effectively detect early-developing tumors is challenging, especially in physiological locations with limited visibility or access. Previously, we reported a sensing platform and methodology to detect biomarker peptides found in urine from ovarian cancer patients. This sensing platform relies on peptide interactions with gold nanoclusters through thiol-mediated linkages; thus, the sensitivity of the biomarker assay is directly related to appropriate redox states of the biomarkers in question. Here, we report on an expansion of the traditional thiol-reactivity assay originally developed by Ellman to include and evaluate a variety of solution modifications that may be used in conjunction with the biomarker-sensing platform. Because biomarker peptides may be isolated from a variety of biological tissues or fluids, depending on the target condition or disease, we screened numerous solution conditions that may be directly used in sample preparation and peptide extraction. The data demonstrate that the assay maintains linearity under these various conditions. The assay was then applied to a variety of models and biomarker peptides and exhibits the expected linear response. These results demonstrate the applicability of the thiol-reactivity assay to biologically derived samples, and the flexibility to ensure sample preparation and treatment will retain the appropriate sample redox conditions to ensure optimal interactions with the biosensor platform. It also facilitates the ability to perform quality control on clinically derived biological samples to ensure appropriate preparations, and concentrations are available for application to the nanopore biosensor platform. Full article

Over the past decade, more than a thousand new psychoactive substances (NPSs) have emerged worldwide. This rapid proliferation of “designer drugs” poses significant challenges for drug control, forensic analysis, and public health. Artificial intelligence (AI) has increasingly been applied to address these challenges in NPS design and analysis. This review provides a comprehensive overview of AI methodologies—including deep learning, generative models, and quantitative structure–activity relationship (QSAR) modeling—and their applications in the synthesis, prediction, and identification of NPSs. We discuss how AI-driven generative models have been used to design novel psychoactive compounds and predict their pharmacological activity, how QSAR models can forecast potency and toxicological profiles, and how machine learning is enhancing analytical chemistry workflows for NPS identification. Special emphasis is placed on mass spectrometry (MS)-based techniques, where AI algorithms (e.g., for spectral prediction and pattern recognition) are revolutionizing the detection and characterization of unknown NPSs. A dedicated section examines the legal and regulatory implications of AI-generated psychoactive substances in the European Union (EU) and United States (USA), highlighting current policies, potential gaps, and the need for proactive regulatory responses. The review concludes with a discussion of the benefits and limitations of AI in this domain and outlines future directions for research at the intersection of AI, analytical chemistry, and drug policy. Full article

The objective of this work is to study the anti-inflammatory effect in vitro and in vivo of microwave (MW) extracts of Thymus algeriensis. The in vitro study was performed by the human red blood cell protection test, while the in vivo study used the carrageenan-induced rat paw edema model. The experimental results were confirmed by a molecular docking calculation. The results indicated that all the microwave extracts have a moderate anti-inflammatory effect, depending on their richness in phenolic compounds. Among the extracts studied, the one obtained at 100 °C for 15 min exhibited the most pronounced anti-inflammatory effect, with an inhibition of 78.52%, which is attributed to its high flavonoid content. In particular, the flavonoids naringin and catechin showed the best affinity for the target protein, with values of −10.3 kcal/mol and −9.2 kcal/mol, respectively, as well as low inhibition constants of 0.028 μM and 0.18 μM. These results indicate that these flavonoids generate interactions that enhance the stability of the target ligand–protein complex, thus contributing to the observed anti-inflammatory effect. Full article

This research introduces a novel synthetic method for introducing highly luminescent silver nanoclusters (AgNCs). The technique relies on coffee Arabica seed extraction (CSE), which is the focus of this study. Our developed and manufactured ecologically friendly approach has enhanced the selectivity of AgNCs for Hg(II) ions. The coffee extract was employed in the synthesis process to stabilize and enhance the quantity of AgNCs generated. Various advanced techniques were used to characterize the AgNCs precisely in their prepared condition concerning size, surface modification, and composition. The fluorescence quenching of the AgNCs was the mechanism via which the CSE-AgNCs reacted to the principal metal ions in the experiment. Using this sensing methodology, a very accurate and selective sensing method is provided for Hg(II) in the dynamic range of 0.117 µM to 1.4 µM, with a limit of detection (LOD) equal to 35.21 nM. Comparative research was conducted to determine how selective CSE-AgNCs are for Hg(II) ions compared to other ions. Consequently, a notable degree of selectivity of AgNCs towards these Hg(II) metal ions was achieved, allowing the sensitive detection of Hg(II) metal ions, even their interfering metal ions, in the environment. AgNCs can detect Hg(II) at acceptable values within the nanomolar range. Based on their characteristics, Hg(II) ions were detected in real samples using CSE-AgNCs. Full article

Tropaeolum majus L. is an edible plant known for its therapeutic and medicinal effects, as it possesses bioactive compounds (polyphenols, glucosinolates, fatty acids) and has various biological activities, which makes it interesting and makes it the research objective of this work. The aim of this study was to extract the phenolic compounds present in the T. majus plant by maceration and ultrasound-assisted extraction techniques using two solvents: 80% ethanol and water. In vitro digestion was performed to see how stable the phenolic components are after digestion. An LC-MS/MS instrument was used to identify and quantify the phenolic components. The highest extraction yield for the T. majus extract was obtained when 80% ethanol was used as the solvent after ultrasound-assisted extraction (32.63 ± 2.28 mg/0.5 g fresh material), while the opposite was true for the T. majus extract when water was used as the solvent and maceration as the technique (21.00 ± 3.26 mg/0.5 g fresh material). However, water extracted more phenolic components for identification. In general, the major compounds before in vitro digestion with commercial enzymes and with 80% ethanol and water as the solvents were p-hydroxybenzoic acid, protocatechuic acid, p-coumaric acid, caffeic acid and chlorogenic acid. After in vitro digestion using both solvents and extraction procedures, the stable phenolic compounds were p-hydroxybenzoic acid (>67%) and p-coumaric acid (>35%). Caffeic acid and quinic acid were not detected after digestion. The stability of certain phenolic components could influence the use of such extracts as dietary supplements with beneficial effects on human health, making them interesting for the general population. Full article

With the rise in global temperatures, it is of great significance to achieve rapid and accurate detection of greenhouse gases, such as carbon dioxide and methane. Raman spectroscopy not only overcomes the weakness of absorption spectroscopy in simultaneously measuring homonuclear diatomic molecules but also enables the simultaneous detection of multiple gases using a single-wavelength laser. However, due to the small Raman scattering cross-section and weak intensity of molecules, its application in gas detection is limited. To enhance the intensity of Raman scattering, this paper designs and constructs a multi-pass enhanced Raman spectroscopy setup. This study focuses on the effects of Raman scattering collection geometry, laser multi-pass patterns, and laser polarization relative to the Raman collection direction on signal intensity. Investigations into Raman scattering collection angles of 30°, 60°, and 90° reveal that the Raman scattering signal intensity increases as the collection angle decreases. Different laser multi-pass patterns also impact the signal, with the near-concentric linear multi-pass pattern found to collect more signals. To minimize the influence of excitation light on the signal, a side collection system is employed. Experiments show that the Raman scattering signal is stronger when the laser polarization is perpendicular to the collection direction. This study achieves overall system performance enhancement through coordinated optimization of multiple physical mechanisms, including Raman scattering collection geometry, laser multi-pass patterns, and laser polarization characteristics. The optimized setup was employed to characterize the laser power dependence for nitrogen, oxygen, and carbon dioxide detection. The results showed that the Raman scattering intensity varied linearly with the laser power of the gases, with linear fitting goodness R² values of 0.9902, 0.9848, and 0.9969, respectively. Finally, by configuring different concentrations of carbon dioxide gas using nitrogen, it was found that the Raman scattering intensity varied linearly with the concentration of carbon dioxide, with a linear fitting goodness R² of 0.9812. The system achieves a CO₂ detection limit of 500 ppm at 200 s integration time, meeting the requirements for greenhouse gas emission monitoring applications. Full article

Electroanalysis has emerged as a critical tool in the pharmaceutical industry, offering versatile and sensitive methods for drug analysis. This review explores the principles, techniques, and applications of electroanalysis in pharmaceuticals, emphasizing its role in drug development, quality assurance, pharmacokinetics, and environmental monitoring. Key electroanalytical methods, including voltammetry, potentiometry, and amperometry, are detailed along with their practical applications, such as detecting active pharmaceutical ingredients, monitoring drug metabolites, and ensuring product stability. Innovations in electrode materials and biosensors have enhanced their sensitivity and specificity, paving the way for advanced drug screening and therapeutic monitoring. Challenges like electrode fouling, selectivity issues, and regulatory constraints are discussed, along with strategies to overcome them. Future trends highlight the integration of nanotechnology, AI, and portable sensors to facilitate real-time analysis and personalized medicine. These advancements position electroanalysis as an indispensable component of modern pharmaceutical research and healthcare. Future perspectives emphasize the integration of nanotechnology and artificial intelligence (AI) to optimize experimental processes and data interpretation. This study also predicts the increased adoption of lab-on-a-chip systems and bioelectrochemical sensors to meet the growing demand for precision medicine and sustainable pharmaceutical practices. These advancements position electroanalysis as a cornerstone of pharmaceutical research, paving the way for more efficient drug development, improved patient outcomes and better environmental management. This comprehensive review underscores the transformative potential of electroanalysis in addressing the evolving challenges of the pharmaceutical industry and provides a foundation for future innovations. This review does not explicitly define the timeframe for the considered advancements. However, it discusses recent technological developments, including innovations in nanostructured electrodes, microfluidic integration, and AI-driven data analysis, indicating a focus on advancements primarily from the last few years, i.e., from 2020 to 2025. Full article

A diagnostic chemical analysis has been performed on a Roman Cippus funebris in precious white marble located close to an ancient Roman road. The Cippus was in good condition but almost completely covered by a black patina, requiring a conservative cleaning intervention. The restorer in charge of the restoration asked us to make a preliminary diagnosis, on the basis of which we could suggest the most appropriate intervention. The Cippus was dedicated to the young Quintus Cornelius Proclianus, who died at the age of 15, by his mother Valeria Calpurnia Scopele. It perfectly fits into the Roman funerary liturgy and also shows an Etruscan-type iconography that seems to confirm the Etruscan Gens of the family and its dating to the 1st century AD. Ion chromatography (IC) analyses were performed to determine anions and cations on solutions obtained from the extraction of salts from the four samples of the Cippus. pH, conductivity, and red-ox potential measures, as well as UV-visible spectra were carried out on the same solutions. A small fragment, spontaneously fallen from the Cippus’ surface, was also observed by optical microscopy (OM) and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS). From the analyses, the dark patina that covered the surface before cleaning turned out to be made of black crusts, that is, smog particles adsorbed on sulfates, but above all, by a layer of microflora. The results allowed us to suggest some conservative interventions. Full article