Volume: 13

Issue: 50

Contents:

This issue of BrJAC contains an Editorial by Prof. Victor G. Mihucz (Eötvös Loránd University, Hungary), an Interview by Prof. José Alberto Fracassi da Silva (Unicamp, Brazil), a Point of View by Prof. Josué Carinhanha C. Santos (UFAL, Brazil), a Letter by Prof. Wendel A. Alves (UFABC, Brazil), one review, and five articles. Readers will also find features on the XX Colacro and the 10th Analítica Latin America Congress, sponsor reports and releases, book notices, and a calendar of events.

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Editorial

 

Prof. Dr. Victor G. Mihucz
Professor at the Eötvös Loránd University, Budapest, Hungary

"It is with great pleasure that I introduce the 50th issue of the Brazilian Journal of Analytical Chemistry, which once again reflects the vitality, diversity, and innovation of our community. The contributions gathered here span fundamental reflections, methodological advances, and applications that resonate with both academic research and industrial practice."

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Interview

 

Professor José Alberto Fracassi kindly granted an interview to BrJAC

Prof. Dr. José Alberto Fracassi da Silva
Associate Professor at the Institute of Chemistry, State University of Campinas, SP, Brazil

"I'm very glad to say that the Analytical Chemistry community in Brazil is very active. I don't think it's an exaggeration to say that each specific area within Analytical Chemistry has Brazilians who are among the leaders in the field. Therefore, I see that scientific research in Analytical Chemistry in Brazil has reached a level of maturity. Perhaps, the focus for the future would be increasing the impact of the research, which can be achieved by establishing of collaborative networks and increasing investments in scientific research in Brazil. I can highlight the successful initiative of the Federal Government regarding the implementation of the National Institutes on Science and Technology (INCTs). I hope for more initiatives of this type."

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Point of View

 

Thimerosal, an Organic Mercury Compound used as a Vaccine Preservative: A real necessity or regulatory inertia? Contributions from analytical chemistry

Prof. Dr. Josué Carinhanha Caldas Santos
Full Professor at the Institute of Chemistry and Biotechnology, Federal University of Alagoas, AL, Brazil

"…The data generated by analytical chemistry, speciation studies, kinetic analyses, stability evaluations, and post-use surveillance not only allow for a more detailed characterization of the toxicological profile of EtHg, but also provide technical support for transitioning to safer and scientifically sound alternatives. Thus, analytical advances cease to function merely as evaluative tools and become true catalysts for change, providing the scientific basis required for regulators and manufacturers to adopt policies and formulations that progressively reduce dependence on mercury compounds in vaccines..."

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Letter

 

Polymeric Microneedles as Analytical Interfaces for Biosensing and Controlled Drug Release: Achievements and Future Challenges

Prof. Dr. Wendel Andrade Alves
Full Professor at the Center for Natural and Human Sciences, Federal University of ABC (UFABC), Santo André, SP, Brazil

"…The future of polymeric microneedles lies in the development of integrated analytical and therapeutic platforms that can operate autonomously and safely for prolonged periods. The convergence of conductive polymers, nanocomposites, and biocompatible hydrogels with emerging technologies, such as microfluidics, data analytics, and artificial intelligence, will enable real-time interpretation of biochemical signals and dynamic therapeutic adjustments. In parallel, the analytical chemistry community plays a central role in ensuring metrological traceability, calibration accuracy, and long-term stability of microneedle-based biosensors, thereby consolidating their reliability in clinical diagnostics..."

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Acknowledgments

 

BrJAC editors are grateful to all those who have reviewed papers in 2025 using significant time and effort to provide constructive inputs.

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Review

Review: Overview of the Greenness' Metrics used to Evaluate Analytical Methods
Amanda Mohr, Brendha Lang Camboim, Andreas Sebastian Loureiro Mendez, Cássia Virginia Garcia, Martin Steppe

The main goal of Green Analytical Chemistry (GAC) is to reduce the use of hazardous chemicals and waste generation in analytical procedures without compromising method performance. Over the years, several metrics tools were introduced to measure the environmental impact and greenness of analytical procedures. In this context, this paper aims to present an overview of the most used GAC metrics in analytical chemistry, highlighting their criteria, advantages, disadvantages, and comparing their applicability. After extensive research, the metrics selected to be addressed were: National Environmental Method Index (NEMI), Analytical Eco-scale, Modified Green Analytical Procedure Index (MoGAPI), and Analytical GREEnness Metric (AGREE). NEMI is one of the oldest GAC metrics, describing the greenness of the method by a simple pictogram. Analytical Eco-Scale is based on subtracting penalty points from a total score of 100 points. MoGAPI uses a pictogram made up of fifteen categories and a total score to display the greenness of the analytical procedure. AGREE is represented as a circular pictogram divided into 12 parts, where each part corresponds to a principle of GAC. Each discussed metric has its own advantages and disadvantages; however, AGREE stands out as the most widely used and comprehensive GAC metric, applicable to several techniques. Although time-consuming, ideally, the best approach is to apply all metrics in combination to gain as much information as possible.

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Articles

Article: Updating of Quantitative Models in Validation and Routine Tests of Comparative Chemical Methods
Omar Djellouli, Eric Rozet, Benamar Dahmani, Philippe Hubert

Nowadays, health and safety requirements are becoming more urgent, through normative and regulatory texts, considering the intense demands of customers from the different sectors of socio-economic activities. Chemical testing must undoubtedly assume a large part of the tasks related to these concerns, despite the delay observed in their metrological concepts, due to the complexity of the chemical and biological samples. Hence, technical and methodological creativity will be well supported, including theoretical revisions and updates of existing methods, in order to overcome the various encountered analytical problems and to fill some frequent lack of metrological tools. In this study, we propose hybrid quantification models, while showing their contributing effects on analytical improvement and decision-making in validation and routine testing of comparative chemical methods. To this end, external calibration plans, with or without a matrix, were established to generate and compare various quantitative models, which make it possible to determine, cleverly, validation and real samples concentrations. The obtained results shed light on the real causes leading to the poor quality that can be found in the obtained validation data. However, highlighted quantitative models show an improvement in both precision and accuracy, which reduce by (5 to 9%) the uncertainty measurement. In addition, these estimates show a comparable quality for routinely tests.


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Article: Optimization and Validation of Ultrasound-Assisted Extraction for Total Phosphorus Analysis in Cane Syrup
Vandressa Alves, Jucimara Kulek de Andrade, Maria Lurdes Felsner

Cane syrup, a nutrient-rich by-product of sugarcane, is valued for its bioactive compounds and mineral content, including phosphorus, a vital macromineral essential for human bone health, enzyme activity, and plant metabolism. Conventional methods for total phosphorus analysis in such viscous matrices face challenges, such as matrix interference, high reagent consumption, and environmental impact. This study optimized and validated an ultrasound-assisted extraction (UAE) method combined with UV-VIS spectrophotometry for determining total phosphorus in cane syrup. UAE parameters were optimized using a simplex centroid mixture design to assess the effects of HNO₃, HCl, and ultrapure water as extraction solvents. UV-VIS spectra revealed that HCl-rich extraction solvents enhanced pigment production via the Maillard reaction, interfering with spectrophotometric detection. In contrast, ternary acid mixtures minimize these effects. The optimal conditions (1.67 mL HNO₃, 2.00 mL HCl, and 1.30 mL H₂O) achieved recovery rates of approximately 100%, without significant matrix interference. The validation of UAE combined with UV-VIS spectrophotometry demonstrated excellent selectivity and linearity (R² > 98.0%), low limits of detection and quantification (0.296 μg g⁻¹ and 0.898 μg g⁻¹, respectively), and good precision (RSD < 11%). The method's accuracy was confirmed through a paired t-test comparison with microwave-assisted digestion (MAD), showing no significant differences (p > 0.05). UAE proved to be more environmentally friendly than MAD, with lower energy consumption (4.17 vs. 62.50 Wh/sample) and reduced reagent usage, as indicated by the AGREEprep metrics (scores: 0.41 vs. 0.30). The total phosphorus content in cane syrup samples varied significantly (11.48–129.54 mg kg⁻¹), influenced by geographical origin and production processes. The validated UAE method provides a fast, cost-effective, and sustainable alternative for phosphorus analysis in complex food matrices, aligning with the principles of green chemistry.

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Article: A Green and Lean Method Certified by NEMI, ESA, AGREE, GAPI and BAGI for the Analysis of Ivermectin in Injection Solution for Veterinary Use
Natália Sabina dos Santos Galvão, Ana Carolina Kogawa

The use of antiparasitics, such as ivermectin (IVE), is extremely important to public health and economy. Quality control and analytical development are necessary to guarantee the efficacy, safety and quality of medicines. The work covered the development and validation of a green and lean method by UV to quantify IVE in injection solution for veterinary. UV methodology using ethanol as a diluent, quartz cuvette and spectrophotometer at 245 nm were used. In order to bring objectivity in relation to the greenness of the proposed method, 5 tools were used: National Environmental Method Index (NEMI), Eco-Scale Assessment (ESA), Analytical GREEnness Metric (AGREE), Green Analytical Procedure Index (GAPI), Blue Applicability Grade Index (BAGI). The proposed method was linear in the range of 6-16 µg mL-1, precise (RSD < 5%), selective and indicative of stability by forced degradation, exact (100.07%) and robust against small and deliberate modifications. NEMI showed the 4 green quadrants, GAPI showed predominantly green and yellow quadrants, ESA, AGREE and BAGI showed scores of 96, 0.82 and 65, respectively. The method is an excellent and lean green option for evaluating final IVE product. It has an environmentally friendly footprint, which can be advantageously employed by pharmaceutical chemical laboratories worldwide.

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Article: Enhanced Microwave-Assisted Digestion Method for Accurate Trace-Level Analysis of Rare Earth Elements in Environmental Matrices
Gabriela S. Caldeira, Pedro C. Evangelista, Bianca D. Pereira, Nicholas E. Bernhard, Mariana M. Lage, Geraldo M. S. Sampaio, Fernando B. Egreja Filho, Claúdia C. Windmöller

Rare Earth Elements (REEs) play an essential role in modern technologies, with soils and sediments often acting as the final repository for REE-containing products. This study evaluates sample preparation methodologies using digestion protocols and triple quadrupole inductively coupled plasma mass spectrometry (ICP-QQQ) for accurate REE quantification in soils, sediments, and rocks. Five digestion protocols—differing in hydrofluoric acid (HF) usage and fluoride interference mitigation (Methods 1, 2, 3, USEPA 3052, and 3051)—were compared, identifying Method 3 as the optimal approach. Method 3, which includes 3.0 mL of HF, 3.5 mL of HCl, 1.5 mL of HNO₃, and boric acid (H₃BO₃) to neutralize fluorides, achieved REE recovery rates exceeding 84% across all certified reference materials (CRMs), including soil (TILL-3, NIST SRM 2709a), sediment (NIST SRM 8704), and rock (ITA-1 Friable Itabirite) samples. This method significantly reduces digestion time from 12 hours to 3 hours, minimizes acid consumption, and enhances sample throughput, offering a highly efficient workflow. In addition, Method 3 demonstrated high precision within a 95% confidence interval, excellent linearity, and minimal matrix interference for all REEs (except scandium). Detection limits (LOD: 0.0025–0.0610 µg g-1) and quantification limits (LOQ: 0.0072–0.1448 µg g-1) were markedly lower than previously reported values, enabling sensitive, trace-level REE analysis in complex environmental matrices. Overall, Method 3 stands out as an efficient, precise, and environmentally sustainable protocol for multi-element analysis, providing a rapid and reliable solution for REE quantification in soils, sediments, and rocks using ICP-MS/MS.

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Article: Comparative Study Between Calcination and Thermogravimetry Techniques in the Quantification of Carbon Black Content in Polymeric Resins
Amanda Aparecida Dill de Souza, João Henrique Zimnoch dos Santos

In the characterization laboratory involving polymeric resins from the petrochemical industry, the carbon black content in polymeric resins is analyzed using two techniques: calcination and thermogravimetric analysis (TGA). In a comparative way, the objective of this study is to verify whether there is a significant difference between the results obtained by these two methods, aiming to reduce the response time of results for customers, with the same quality and accuracy and improvements in matters of Health and Safety Environment (HSE) such as, for example, the exposure of analysts to high temperatures used in the microwave oven used in calcination. In the experimental conditions, the calcination technique obtained a higher uncertainty value compared to TGA, but the results showed precision and accuracy in both techniques. Furthermore, the method developed by TGA provided a 175% increase in productivity and advancement for the analysts safety involved in carrying out the activities as it has low risks when compared to calcination.

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Features

The 10th Analítica Latin America Congress Consolidates Brazil as a Scientific Hub

From September 23 to 25, 2025, the 10th Analítica Latin America (ALA) Congress was held in São Paulo, bringing together around 90 participants and reaffirming its position as the leading scientific meeting on analytical chemistry in Latin America. Held alongside the ALA Fair—the largest event in the analytical chemistry sector in Latin America—the ALA Congress fostered dialogue among academia, industry, and research institutes in an environment focused on innovation, sustainability, and technological development.

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COLACRO XX Brings Together 450 Participants and Becomes One of the Most Significant Events in Latin American Chromatography

The COLACRO XX, held from October 28 to 31, 2025, in Campos do Jordão (SP, Brazil), marked one of the most relevant editions in its history. With 450 participants from various countries across Latin America, Europe, and North America, the event has reaffirmed its strategic role in advancing separation techniques and sample preparation. The organizer of the event—Professor Fernando Lanças (IQSC-USP), emphasized that the congress has fulfilled its mission of promoting scientific excellence and integration among academic communities.

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Sponsor Technical Applications and Instrumentation Updates

The content in this section is the sole responsibility of the sponsors

Sponsor Reports

Pharma materials study: GC-MS identification of extractables and leachables from elastomer material
Bénédicte Gauriat, Isabelle Froger, Damien Chevaillier, Hans-Joachim Huebschmann
Thermo Scientific

This application note describes a part of an extractable analysis of an elastomeric plunger considered for potential use in a dental injectable cartridge using different extraction techniques, derivatization and HS analysis by single quadrupole GC-MS. A parallel classical flame ionization detection (FID) channel was configured for use in a future routine method, if required.

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Integration of rare earth elements into a novel ICP-MS method for environmental analysis
Tomoko Vincent
Thermo Scientific

The goal of this application note is to demonstrate the suitability of the Thermo Scientific™ iCAP™ TQe ICP-MS using a single measurement mode for rare earth elements (REE) in a variety of environmental and geological samples. It describes how interference free, low level analysis of REE can be integrated into a fast, sensitive, and robust ICP-MS method for the analysis of different water samples.

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Microwave-assisted acid digestion of geological samples for elemental quantification on ICP-MS: Exotic rocks with rare and resistant minerals
Milestone

This document presents a four-step protocol designed for the complete dissolution of exotic rocks samples that contain rare and refractory minerals (Pegmatites, ores, hydrothermally altered rocks, carbonatites), significantly reducing the time required for elemental analysis sample preparation.

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Sponsor Releases

ISQ™ 7610 Single Quadrupole GC-MS

Produce results more rapidly and experience unstoppable efficiency in your analysis with the Thermo Scientific™ ISQ™ 7610 Single Quadrupole GC-MS system. Simplified operation, automated workflows, and extended dynamic range deliver consistent results from system to system in every laboratory.

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Triple quadrupole ICP-MS with advanced interference removal

The Thermo Scientific iCAP MTX Triple Quadrupole ICP-MS system is a high-performance instrument that can be integrated into the most challenging analysis workflows. The system gives you confidence in a streamlined sample pathway that consistently provides highly accurate results.

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ultraWAVE 3 Taking Productivity and Performance to New Heights

The new Milestone ultraWAVE 3 is the latest generation of SRC technology that further elevates the value of this technology for elemental analysis in terms of performance, time, workflow, and cost of ownership.

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Releases

Pittcon Conference & Expo

Pittcon is a friendly, welcoming environment where analytical chemists at all professional levels meet. Pittcon is a platform for sharing ideas and cooperating to form new ones. At Pittcon, you will find that spark that drives your research, your career, and above all, your scientific perspective forward.

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SelectScience® Pioneers online Communication and Promotes Scientific Success

SelectScience® informs through trusted lab product reviews, virtual events, thought-leading webinars, features on hot scientific topics, eBooks and more, independent online publisher SelectScience® provides scientists across the world with vital information about the best products and techniques to use in their work.

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CHROMacademy is the leading provider of eLearning for analytical science

For over 10 years, CHROMacademy has increased knowledge, efficiency and productivity across all applications of chromatography.

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BrJAC – Brazilian Journal of Analytical Chemistry