Analytica

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

Green analytical chemistry represents a transformative approach to analytical science, emphasizing sustainability and environmental stewardship while maintaining high standards of accuracy and precision. This review highlights recent innovations in green analytical chemistry, including the use of green solvents, such as water, supercritical carbon dioxide, ionic liquids, and bio-based alternatives, as well as energy-efficient techniques like microwave-assisted, ultrasound-assisted, and photo-induced processes. Advances in green instrumentation, including miniaturized and portable devices, and the integration of automation and chemometric tools, have further enhanced efficiency and reduced the environmental footprint of analytical workflows. Despite these advancements, challenges remain, including the need to balance analytical performance with eco-friendliness and the lack of global standards to measure and promote sustainable practices consistently. However, the future of green analytical chemistry looks promising, with emerging technologies like artificial intelligence and digital tools offering new ways to optimize workflows, minimize waste, and streamline analytical processes. By focusing on these areas, green analytical chemistry is transforming analytical methodologies into tools that not only achieve high performance but also align with global sustainability goals. This review underscores how green analytical chemistry is more than just a scientific discipline, but a pathway for reducing the ecological impact of analytical processes while driving innovation in science and industry. With the continued commitment to research, collaboration, and the adoption of cutting-edge technologies, green analytical chemistry has the potential to shape a greener and more sustainable future for analytical chemistry and its diverse applications. Full article

This study investigated the effect of surface treatments on the electrochemical performance of 3D-printed electrodes for versatile applications. The conductive filament was obtained from a mixture of polylactic acid (PLA) and carbon black (CB) at a 7:3 ratio (PLA/CB) dispersed in acetic acid and dichloroethane (3:1) medium. The treatments used were HNO₃, NaOH, DMF (immersion for 30, 30, and 15 min, respectively), and electrochemical activation (amperometry 150 s, 1.8 V). In general, the treatments allow greater exposure of the conductive material and active sites present on the sensor surface. This was confirmed using cyclic voltammetry and electrochemical impedance spectroscopy. The analyses were conducted with a 0.10 M KCl solution containing the redox pair ferricyanide/ferrocyanide 5.00 mmol L⁻¹. Based on the results obtained, the electroactive area, kinetic constant and resistance to electron transfer were determined for each treatment. The treatment in basic medium stood out as the treatment that was most appropriate for the device used in this work. The device was also tested for its potential in the analysis of acetaminophen, demonstrating satisfactory results permitting the application of 3D-S_Basic in the analysis of acetaminophen. Full article

GLANCE (Graphical Layout Tool for Analytical Chemistry Evaluation) is an innovative and adaptable free, editable template specifically designed to help researchers visually summarize their analytical chemistry methods in a structured and clear manner. It provides an accessible solution to the challenge of presenting complex scientific data, offering a significant advantage over traditional reporting methods, which often lack visual clarity. This is crucial because no previous tool has been developed to summarize analytical methods in such a comprehensive and concise visual format, significantly enhancing the process of gathering and presenting key information, particularly in review articles. The GLANCE template (bit.ly/409cwDd) is composed of twelve distinct attributes, each targeting critical aspects of method development (novelty, analytes, sample preparation, reagents, instrumentation, method validation, matrix effects and recoveries, application to real samples, analytical metrics, main results, limitations, and additional information). By filling out each block with keywords or short phrases, authors can provide a concise yet thorough overview of their method. Once completed, the template can be easily downloaded and included in scientific articles. This straightforward integration enhances both the clarity and accessibility of publications, providing the scientific community with a quick snapshot of the principal features of research. Full article

Serial femtosecond crystallography (SFX) using X-ray free-electron lasers (XFELs) enables the determination of biological and chemical structures without radiation damage. In SFX experiments, a sample delivery system is essential for delivering numerous crystals to the X-ray interaction point in a serial and stable manner. Among the various sample delivery methods, the fixed-target (FT) sample delivery system is straightforward and widely used for collecting SFX data due to its advantages of low sample consumption and reduced physical damage to crystals during data collection. Here, we review the development of the FT sample delivery system for SFX with the Pohang Accelerator Laboratory X-ray free-electron laser (PAL-XFEL). The specifications and operational conditions of the FT-SFX sample chamber are described. The design, specifications, and applications of the one- and two-dimensional FT sample holders developed for SFX with the PAL-XFEL are also detailed. Furthermore, the applications of each FT sample delivery system are discussed. This review not only provides valuable information on the FT system used in SFX experiments with the PAL-XFEL but also offers insights into the development of FT sample delivery systems. Full article

Neonatal jaundice affects over 80% of newborns globally, posing significant health risks if untreated. Current diagnostic methods either lack accuracy or are prohibitively expensive, limiting accessibility in low-resource settings. This study presents a cost-effective, wearable device for non-invasive bilirubin monitoring based on forehead skin tone analysis. The device, comprising a TCS34725 color sensor and ESP32-C3 microcontroller, offers real-time bilirubin predictions validated against standard clinical methods. Calibration ensures reproducibility across devices, with recovery rates of 91–107%, meeting analytical validation standards. This innovation has the potential to revolutionize neonatal care by providing accessible, sustainable, and accurate monitoring, especially in underserved regions. Full article

Serial crystallography (SX) determines the crystal structures of target molecules at room temperature with minimal radiation damage. During SX data collection, the stable delivery of many microcrystals to the X-ray interaction point is crucial for efficient sample consumption and effective beamtime usage. Most microcrystal delivery techniques for SX require sophisticated devices or specialized techniques, which can be challenging for data collection. This review introduces a straightforward method that delivers microcrystal samples in SX experiments using a commercially available syringe and syringe pump. This method does not require specialized skills for sample delivery and can be tested in the laboratory prior to SX data collection at the beamline. Advantages and disadvantages of this method are also discussed, along with various application cases. This straightforward sample delivery approach is concluded to facilitate efficient SX data collection. Full article

In recent years, Thailand’s agriculture sector has seen a significant rise in pesticide usage due to its vital role in the economy and global food trade. However, the uncontrolled use of pesticides poses severe health and environmental risks. This research focuses on the detection of pesticide residues, particularly carbaryl and paraoxon-ethyl, which are prevalent due to their high efficacy in pest control but pose neurological health risks by inhibiting acetylcholinesterase (AChE) activity, potentially impacting human health. The developed method assesses pesticide concentration by measuring changes in the CIE-LAB color space using a smartphone camera. Testing several concentrations (0.2, 0.6, and 1.0 ppm) over time revealed significant differences via ANOVA (F = 32.8, p < 0.001) and a strong linear relationship with R² values from 0.9129 to 0.9973 through regression analysis. Additionally, principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) were utilized to further understand the relationship between color changes and pesticide type and concentration. PCA showed that the L* and b* values contributed most to explaining the variance in the data (96.24%), while PLS-DA provided classification models. These strong linear relationships between pesticide concentration and colorimetric changes showcase the method’s accuracy and potential for on-site pesticide monitoring in agricultural produce, emphasizing technological advancements in sustainable agriculture practices. This research presents encouraging findings from an inexpensive and straightforward method for detecting pesticide residues, suggesting that a specialized mobile application could enhance the implementation of the proposed system. Full article

The development of screen-printed electrochemical sensors represents a rapidly expanding research field with great potential for applications in the rapid and sensitive determination of drugs in complex matrices. This work presents a review of the state-of-the-art examples of this technology, focusing on its application in real matrices such as water, pharmaceutical formulations, and biological fluids. We discuss the main materials used in developing conductive inks, highlighting their properties and influence on sensor performance. The characterization of materials and sensors is crucial to ensure the reproducibility and reliability of results. Additionally, we address the challenges associated with the application of these sensors in complex matrices, such as interferences from other components and the need for sample pretreatment. Finally, we present future perspectives for developing screen-printed electrochemical sensors, with an emphasis on new technologies and materials that can improve the sensitivity, selectivity, and stability of these devices. Full article

The role of pipecolic acid (Pip) in plant immune responses, particularly against bacterial wilt pathogens, is significant. This research aimed to understand the interaction between plant defense-responsive enzymes and Pip by analyzing methanolic extracts from different treatments of tolerant (GAT5) and susceptible (GT2) tomato cultivars. LC-MS analysis demonstrated that the foliar application of Pip significantly influenced tomato metabolites, especially in bacterial wilt-infected plants, with a more pronounced effect in tolerant varieties. Principal component analysis (PCA) revealed that Pip-treated plants of tolerant varieties exhibited better coordinated metabolome profiles than those of susceptible varieties. Notable variations were observed in the levels of specialized metabolites, such as salicylic acid (SA), N-hydroxy pipecolic acid (NHP), and Pip, which are essential for producing defense compounds. Molecular docking studies further explored Pip’s interactions with key plant enzymes involved in defense mechanisms and showed that Pip acts as an effective organic inducer of systemic acquired resistance (SAR). These findings highlight Pip’s potential as a natural agent for enhancing plant tolerance to pathogens, offering promising implications for agricultural practices and improving crop resilience against diseases. This study enhances our understanding of Pip’s role in plant defense and provides a foundation for developing Pip-based strategies for sustainable agriculture. Full article

Corrosion is a critical industrial problem. To solve this problem, the present research analyzed the influence of corrosive media on the efficiency of a guayusa inhibitor. Therefore, guayusa extract was obtained, and five groups of ASTMS A36 steel test tubes were prepared, each with variable extract concentrations (200 ppm, 400 ppm, 600 ppm, 800 ppm, and 1000 ppm) that were exposed to different corrosive media (5% NaCl, 5% NaCl + acetic acid, 1% HNO₃, and 10% HNO₃). The results obtained were compared to determine the percentage efficiency of the inhibitor in each of the corrosive media. This study provides a detailed understanding of how the corrosive environment influences the effectiveness of a guayusa inhibitor, which is used as a green inhibitor for the first time, allowing its viability and performance to be assessed under various conditions. Full article

Substituted phenols, including chlorophenols, are important analytes, particularly in the context of environmental analysis. Chlorophenols are formed during the disinfection of drinking water by chlorination and are important water pollutants. Gas chromatography–mass spectrometry (GC-MS) is an important method for the analysis of chlorophenols. Retention indices are used in GC-MS analysis to improve the accuracy of identification. Our research reveals that the retention indices currently available for substituted phenols are erroneous in a number of cases. We report reliable retention index values for pentafluorophenol, 5-methoxy-2-nitrophenol, 4-cyanophenol (stationary phase: 5%-phenyl-polymethylsiloxane), 3-methoxyphenol, 2-chlorophenol, 3-chlorophenol, 4-chlorophenol, 2,3-dichlorophenol, 2,5-dichlorophenol, 2,6-dichlorophenol, 3,4-dichlorophenol, 3,5-dichlorophenol, 2,3,5-trichlorophenol, 2,3,6-trichlorophenol, 2,4,5-trichlorophenol, and 2,4,6-trichlorophenol (stationary phase: polyethylene glycol modified with 2-nitroterephthalic acid). The structures of the standard samples were confirmed, and measurements were performed under various conditions. The analysis of the causes of the incorrect records appearing in the well-known NIST database was also carried out. Full article

Saquinavir is a drug used as an HIV treatment, with recent reports of new uses. It has poor aqueous solubility and very low oral bioavailability. However, when prepared in a eutectic mixture with the natural bioenhancer, piperine, it demonstrated improvements in these drawbacks. Therefore, considering that EMs can be easily produced and scaled-up, it could potentially be used in new pharmaceutical formulations. For this purpose, an analytical method capable of quantifying SQV in the presence of PIP is required for quality control purposes. In this context, UV–Vis equipment is simpler to use and cheaper than HPLC, and it is commonly available in most laboratories. Therefore, a derivative spectrophotometry method at 245 nm was developed and validated to quantify SQV. The method showed good linearity from 0.5 to 100.0 mg/L, with a limit of detection and limit of quantification of 0.331 mg/L and 0.468 mg/L, respectively. Furthermore, it was precise, accurate, and demonstrated good specificity up to a 1:4.3 SQV:PIP ratio. Consequently, the results demonstrate that the method can be employed for SQV quantification in the presence of PIP as an economical and simple technique. This contribution could be the basis for a quality control technique for these types of products. Full article

We report a workflow and a software description for digital image colorimetry aimed at obtaining a quantitative dose–response curve and the minimal inhibitory concentration in the Resazurin Microtiter Assay (REMA) test of the activity of antimycobacterial drugs. The principle of this analysis is based on the newly established correspondence between the intensity of the ${\mathrm{a}}^{*}$ channel of the CIE L*a*b* colour space and the concentration of resorufin produced in the course of this test. The whole procedure can be carried out using free software. It has sufficiently mild requirements for the quality of colour images, which can be taken by a typical smartphone camera. Thus, the approach does not impose additional costs on the medical examination points and is widely accessible. Its efficiency is verified by applying it to the case of two representatives of substituted 2-(quinolin-4-yl) imidazolines. The direct comparison with the data on the indicator’s fluorescence obtained using a commercial microplate reader argues that the proposed approach provides results of the same range of accuracy on the quantitative level. As a result, it would be possible to apply the strategy not only for new low-cost studies but also for expanding databases on drug candidates by quantitatively reprocessing existing data, which were earlier documented by images of microplates but analysed only qualitatively. Full article

Boron nitride nanostructures (BNNs), including nanotubes, nanosheets, and nanoribbons, are renowned for their exceptional thermal stability, chemical inertness, mechanical strength, and high surface area, making them suitable for advanced material applications. Metal–organic frameworks (MOFs), characterized by their porous crystalline structures, high surface area, and tunable porosity, have emerged as excellent candidates for gas adsorption and storage applications, particularly in the context of hydrogen. This paper explores the synthesis and properties of BNNs and MOFs, alongside the innovative approach of integrating BNNs within MOFs to create composite materials with synergistic properties. The integration of BNNs into MOFs enhances the overall thermal and chemical stability of the composite while improving hydrogen sensing and storage performance. Various synthesis methods for both BNNs and MOFs are discussed, including chemical vapor deposition, solvothermal synthesis, and in situ growth, with a focus on their scalability and reproducibility. Furthermore, the mechanisms underlying hydrogen sensing and storage are examined, including physisorption, chemisorption, charge transfer, and work function modulation. Electrochemical characterization techniques, such as cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge–discharge, are used to analyze the performance of BNN-MOF systems in hydrogen storage and sensing applications. These methods offer insights into the material’s electrochemical behavior and its potential to store hydrogen efficiently. Potential industrial applications of BNN-MOF composites are highlighted, particularly in fuel cells, hydrogen-powered vehicles, safety monitoring in hydrogen production and distribution networks, and energy storage devices. The integration of these materials can contribute significantly to the development of more efficient hydrogen energy systems. Finally, this study outlines key recommendations for future research, which include optimizing synthesis techniques, improving the hydrogen interaction mechanisms, enhancing the stability and durability of BNN-MOF composites, and performing comprehensive economic and environmental assessments. BNN-MOF composites represent a promising direction in the advancement of hydrogen sensing and storage technologies, offering significant potential to support the transition toward sustainable energy systems and hydrogen-based economies. Full article

This study describes the development of an optical-based surface plasmon resonance (SPR) aptasensor for the detection of cocaine. The aptasensor was prepared by first attaching gold nanoparticles to a clean SPR chip surface, followed by the addition of an aptamer to create a modified surface. This surface was characterized using contact angle and atomic force microscopy, revealing surface roughness values of 0.28 nm and 28.12 nm for the blank and modified surfaces, respectively. The detection of cocaine was carried out in the concentration range of 1 ng/mL to 1000 ng/mL, with a detection time of approximately 8 min and a cocaine limit of detection (LOD) of 0.43 ng/mL. Repeatability studies were conducted, and the stability of the signal response was examined at a concentration of 200 ng/mL. Adsorption isotherm models, including Scatchard, Langmuir, and Freundlich models, were calculated to assess the surface homogeneity of the SPR aptasensor chip, with the results indicating compatibility with the Langmuir isotherm model. Full article