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  • Open Access Icon
  • Research Article
  • 10.3390/analytica6030033
Rapid and Efficient Magnetic Nanoparticle-Based Method for Cd Determination in Brazilian Cachaça Using Flame Atomic Absorption Spectrometry
  • Sep 8, 2025
  • Analytica
  • Saulo Alves De Souza + 6 more

The contamination of food and beverages with heavy metals, such as Cd, presents significant health risks, underscoring the need for reliable and sensitive analytical methods. This study introduces the development of a rapid, cost-effective, and environmentally friendly method for Cd determination in cachaça, a traditional Brazilian sugarcane spirit. Magnetic nanoparticles (Fe3O4) functionalized with tetraethyl orthosilicate are synthesized and employed as adsorbents in a dispersive magnetic solid-phase extraction procedure. The extracted Cd is quantified using flame atomic absorption spectrometry. A full factorial experimental design is used to optimize key parameters, including the sorbent mass, adsorption time, desorption time, and acid concentration. The method demonstrates excellent analytical performance, with a linear calibration range (R2 = 0.99), detection limit of 0.0046 mg L−1, and quantification limit of 0.0200 mg L−1. Moreover, validation results show high precision (coefficient of variation < 9.10%) and accuracy (recovery rates between 92.00% and 120.00%). When analyzing commercial cachaça samples, cadmium was detected in all five specimens. Notably, in one sample the cadmium concentration exceeded Brazil’s maximum permissible limit of 0.0200 mg kg−1, underscoring the importance of this work for ensuring food safety. The proposed method offers a sensitive, reproducible, and sustainable approach for analysis of potentially toxic trace metals in alcoholic beverages, reinforcing its potential for routine monitoring and regulatory compliance.

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  • Research Article
  • Cite Count Icon 1
  • 10.3390/analytica6030032
Phenolic Profiling of Merlot Wines from Albania: Influence of Geographical Origin and Vintage Assessed by LC-DAD-ESI-MS/MS
  • Sep 5, 2025
  • Analytica
  • Dritan Topi + 4 more

Merlot red wines rank among the most distinguished varietals globally. This study aimed to characterize the phenolic compound profiles of Merlot wines and assess the influence of geographical origin and vintage on samples from two Albanian wine regions. Using liquid chromatography coupled with tandem mass spectrometry, a total of 31 phenolic compounds were identified and quantified. These were classified into hydroxybenzoic acids and flavan-3-ols (13 compounds), phenolic acids (9), flavonols (5), and stilbenoids (4). The total phenolic content ranged from 294 mg L−1 in wines from the Mati–Mirdita region to 480 mg L−1 in those from the Durrës–Kavaja region, demonstrating significant regional variation. Notably, the hydroxybenzoic acids and flavan-3-ols exhibited the most pronounced differences, with gallic acid concentrations varying from 123 mg L−1 (Mati–Mirdita) to 170 mg L−1 (Durrës–Kavaja). Both regions’ wines were rich in catechin, epicatechin, procyanidin derivatives, trans-caftaric acid, and ethyl gallate. However, procyanidins were found in higher concentrations in the Mati–Mirdita wines, while other phenolics were more abundant in Durrës–Kavaja samples. These findings underscore the influence of geographical and climatic factors on phenolic composition, offering a robust chemical fingerprinting approach for assessing wine authenticity and quality.

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  • Research Article
  • 10.3390/analytica6030031
Multi-Modal Characterization of Wheat Bread Enriched with Pigweed and Purslane Flour Using Colorimetry, Spectral Analysis, and 3D Imaging Techniques
  • Sep 2, 2025
  • Analytica
  • Angel Nikolov + 4 more

The growing demand for functional bakery products necessitates research on the enrichment of wheat bread with pigweed (Amaranthus spp.) and purslane (Portulaca oleracea) flour. Although these plant-based raw materials offer nutritional and environmental benefits, their inclusion in wheat bread formulations poses challenges in the creation of formulations that may compromise the sensory and structural qualities of the final product. The main objective of this work is to systematically determine the optimal amounts of these alternative flour using multimodal bread characterization techniques that include physicochemical, organoleptic, geometric, and optical evaluations, supported by advanced data reduction techniques and regression models. A total of 70 features were analyzed and reduced to 22 for pigweed flour and 15 for purslane flour informative features. Predictive models (R2 = 0.85 for pigweed flour, R2 = 0.84 for purslane flour) were developed to optimize the inclusion of alternative flour, resulting in appropriate concentrations of 3.69% for pigweed flour and 7.13% for purslane flour. These formulations balance improved nutritional profiles with acceptable sensory and structural properties. The results obtained not only complement the potential of pigweed and purslane as sustainable functional raw materials but also demonstrate the efficacy of an automated, image-based approach to formulating recipes in food manufacturing.

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  • Research Article
  • Cite Count Icon 1
  • 10.3390/analytica6030029
Rapid Spectroscopic Analysis for Food and Feed Quality Control: Prediction of Protein and Nutrient Content in Barley Forage Using LIBS and Chemometrics
  • Aug 28, 2025
  • Analytica
  • Jinan Sabsabi + 7 more

Rapid and accurate assessment of nutritional quality, particularly crude protein content and essential nutrient concentrations, remains a major challenge in the food and feed industries. In this study, laser-induced breakdown spectroscopy (LIBS) was combined with advanced chemometric modeling to predict the levels of crude protein and key macro- and micronutrients (Ca, Mg, K, Na, Fe, Mn, P, Zn) in 61 barley forage samples composed of whole aerial plant parts ground prior to analysis. LIBS offers a compelling alternative to traditional analytical methods by enabling real-time analysis with minimal sample preparation. To minimize interference from atmospheric nitrogen, nitrogen spectral lines were excluded from the protein calibration model in favor of spectral lines from elements biochemically associated with proteins. We compared the performance of Partial Least Squares (PLSR) regression and Extreme Learning Machine (ELM) using fivefold cross-validation. ELM outperformed PLS in terms of prediction, achieving a coefficient of determination (R2) close to 1 and a ratio of performance to deviation (RPD) exceeding 2.5 for proteins and several nutrients. These results underscore the potential of LIBS-ELM integration as a robust, non-destructive, and in situ tool for rapid forage quality assessment, particularly in complex and heterogeneous plant matrices.

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  • Research Article
  • 10.3390/analytica6030028
Study of Sorption of Chlortetracycline Hydrochloride on Zirconium-Based Metal–Organic Framework Followed by Determination by UV-Vis Detection
  • Aug 20, 2025
  • Analytica
  • Julia D Bryantseva + 3 more

The reaction of zirconium tetrachloride with 2-amino-1,4-benzenedicarboxylic acid in N,N-dimethylformamide with the addition of HCl leads to the formation of zirconium 2-amino-1,4-benzenedicarboxylate. Zirconium 2-amino-1,4-benzenedicarboxylate was characterized by elemental analysis, infrared spectrometry, X-ray diffraction, scanning electron microscopy, and volumetric nitrogen adsorption/desorption. The sample has a constant porosity with an average pore diameter of 7.97 nm and both microporous and mesoporous structure with a large surface area (820 m2/g) corresponding to the type IV adsorption. Zirconium 2-amino-1,4-benzenedicarboxylate was used for solid-phase extraction (SPE) of chlortetracycline hydrochloride from the aqueous solution. The obtained results confirmed the possibility of using the proposed analytical technique as a new, convenient approach to the extraction of chlortetracycline hydrochloride from industrial or other wastewaters, where such substance is contained in insignificant concentrations and its determination requires expensive and complex equipment. In the future, this method can be used not only for the effective removal of pollutants from industrial wastewater with subsequent regeneration of the sorbent, but also as a sample-preparation method for concentrating chlortetracycline hydrochloride from dilute solutions with its subsequent elution and analysis by available methods, for example, spectrophotometry, since the limit of detection is 0.06 mg/L. Experimental data are described by the isotherm of SPE (R2 = 0.998–0.999) and show the ability of zirconium 2-amino-1,4-benzenedicarboxylate to extract up to 578 mg/g of sorbent at 5 °C under optimal conditions.

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  • Research Article
  • Cite Count Icon 10
  • 10.3390/analytica6030025
Stability Toolkit for the Appraisal of Bio/Pharmaceuticals’ Level of Endurance (STABLE) as a Framework and Software to Evaluate the Stability of Pharmaceuticals
  • Jul 18, 2025
  • Analytica
  • Fotouh R Mansour + 2 more

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.

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  • Research Article
  • 10.3390/analytica6030024
Surface Modification of Poly(butyl methacrylate) with Sulfomethylated Resorcinarenes for the Selective Extraction of Dichromate Ion in Aqueous Media
  • Jul 17, 2025
  • Analytica
  • Cielo Urquijo + 1 more

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.

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  • Research Article
  • 10.3390/analytica6030023
Derivatizing Agent Selection for Hydrophilic Lysine- and Arginine-Containing Tetradecapeptide Analysis in Human Plasma by RP HPLC-MS/MS
  • Jul 10, 2025
  • Analytica
  • Margarita A Tokareva + 5 more

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.

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  • Research Article
  • 10.3390/analytica6030022
Freeze-Drying as a Stabilization Strategy for Natural Dyes Derived from Lawsonia inermis L. and Indigofera suffruticosa
  • Jul 9, 2025
  • Analytica
  • Valvanuz Cahuantzi + 5 more

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.

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  • Research Article
  • Cite Count Icon 2
  • 10.3390/analytica6020021
Multi-Element Determination in Wild and Cultivated Edible Mushrooms from the Brazilian Atlantic Forest Using Microwave-Induced Plasma Optical Emission Spectrometry (MIP OES)
  • Jun 4, 2025
  • Analytica
  • Eliabe Sousa Da Silva + 8 more

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.