Analytica, Volume 6, Issue 1 (March 2025) – 11 articles

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