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Journal = Separations
Section = Analysis of Food and Beverages

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14 pages, 4700 KiB  
Article
Pilot-Scale Phycocyanin Extraction by the Green Two-Step Ultrasound-Based UltraBlu Process
by Rosaria Lauceri, Melissa Pignataro, Antonio Giorgi, Antonio Idà and Lyudmila Kamburska
Separations 2025, 12(8), 194; https://doi.org/10.3390/separations12080194 - 25 Jul 2025
Viewed by 110
Abstract
Phycocyanin is a natural, non-toxic, blue pigment-protein with many commercial applications. Its exploitation in various biotechnological sectors strongly depends on its purity grade (P). Phycocyanin is largely used in food industry where a low purity grade is required, while its widespread use in [...] Read more.
Phycocyanin is a natural, non-toxic, blue pigment-protein with many commercial applications. Its exploitation in various biotechnological sectors strongly depends on its purity grade (P). Phycocyanin is largely used in food industry where a low purity grade is required, while its widespread use in sectors requiring a higher purity is hampered by the cost of large-scale industrial production. Industry, in fact, needs simple, easily scalable and cost-effective procedures to ensure sustainable production of high-quality pigment. In this work we applied the innovative two-step ultrasound-based process UltraBlu to the pilot-scale production of phycocyanin. A total of 50 L of biomass suspension of commercial Spirulina were processed in batch mode. The pigment extract was obtained in one day, including the biomass harvesting. Food/cosmetic grade (P = 1.41–1.76) and a good yield (Y = 59.2–76.1%) were achieved. The initial results obtained suggest that UltraBlu can be an effective scalable process suitable to produce phycocyanin also on an industrial scale. Full article
(This article belongs to the Special Issue Application of Sustainable Separation Techniques in Food Processing)
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14 pages, 1840 KiB  
Article
Volatilomic Fingerprint of Tomatoes by HS-SPME/GC-MS as a Suitable Analytical Platform for Authenticity Assessment Purposes
by Gonçalo Jasmins, Tânia Azevedo, José S. Câmara and Rosa Perestrelo
Separations 2025, 12(8), 188; https://doi.org/10.3390/separations12080188 - 22 Jul 2025
Viewed by 158
Abstract
Tomatoes are globally esteemed not only for their nutritional value but also for their complex and appealing aroma, a key determinant of consumer preference. The present study aimed to comprehensively characterise the volatilomic fingerprints of three tomato species—Solanum lycopersicum L., S. lycopersicum [...] Read more.
Tomatoes are globally esteemed not only for their nutritional value but also for their complex and appealing aroma, a key determinant of consumer preference. The present study aimed to comprehensively characterise the volatilomic fingerprints of three tomato species—Solanum lycopersicum L., S. lycopersicum var. cerasiforme, and S. betaceum—encompassing six distinct varieties, through the application of headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS). A total of 55 volatile organic compounds (VOCs) spanning multiple chemical classes were identified, of which only 28 were ubiquitously present across all varieties examined. Carbonyl compounds constituted the predominant chemical family, with hexanal and (E)-2-hexenal emerging as putative key contributors to the characteristic green and fresh olfactory notes. Notably, esters were found to dominate the unique volatile fingerprint of cherry tomatoes, particularly methyl 2-hydroxybenzoate, while Kumato and Roma varieties exhibited elevated levels of furanic compounds. Multivariate statistical analyses, including principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA), demonstrated clear varietal discrimination and identified potential aroma-associated biomarkers such as phenylethyl alcohol, 3-methyl-1-butanol, hexanal, (E)-2-octenal, (E)-2-nonenal, and heptanal. Collectively, these findings underscore the utility of volatilomic fingerprint as a robust tool for varietal identification and quality control within the food industry. Full article
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11 pages, 846 KiB  
Article
Application of the Precolumn Derivatization Reagent CIM-C2-NH2 for Labeling Carboxyl Groups in LC-MS/MS Analysis of Primary Organic Acids in Japanese Sake
by Mayu Onozato, Haruna Uchida, Misaki Ono, Mikoto Koishi, Maya Oi, Maho Umino, Tatsuya Sakamoto and Takeshi Fukushima
Separations 2025, 12(7), 186; https://doi.org/10.3390/separations12070186 - 16 Jul 2025
Viewed by 244
Abstract
Japanese sake, a traditional alcoholic beverage, contains several organic acids that may contribute to its sour taste. To identify these, a precolumn derivatization reagent, benzyl 5-(2-aminoethyl)-3-methyl-4-oxoimidazolidine-1-carboxylate (CIM-C2-NH2), developed for labeling carboxyl groups, was synthesized and applied to liquid chromatography–tandem [...] Read more.
Japanese sake, a traditional alcoholic beverage, contains several organic acids that may contribute to its sour taste. To identify these, a precolumn derivatization reagent, benzyl 5-(2-aminoethyl)-3-methyl-4-oxoimidazolidine-1-carboxylate (CIM-C2-NH2), developed for labeling carboxyl groups, was synthesized and applied to liquid chromatography–tandem mass spectrometry (LC-MS/MS) analysis of organic acids in six commercial sake samples. The majority primarily contained lactic acid (LA), and dicarboxylic acids, such as succinic acid (SA), malic acid (MA), and citramalic acid (CMA). The organic acid concentrations and compositions in the sake differed among brands. Notably, both l- and d-forms of LA were detected in all samples, while only d-CMA was present. To estimate the total acidic content, neutralization titration with sodium hydroxide was performed. In four of the six samples, titration results closely matched LC-MS/MS data, suggesting that l-LA, d-LA, SA, MA, and d-CMA were the primary contributors for the sour taste in these sakes. The discrepancy between titration and LC-MS/MS data for the other samples was attributed to the presence of other organic acids, which will be investigated in future studies. Full article
(This article belongs to the Section Analysis of Food and Beverages)
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16 pages, 1369 KiB  
Article
Optimized Ethyl Chloroformate Derivatization Using a Box–Behnken Design for Gas Chromatography–Mass Spectrometry Quantification of Gallic Acid in Wine
by Sofia Botta, Roberta Piacentini, Chiara Cappelletti, Alessio Incocciati, Alberto Boffi, Alessandra Bonamore and Alberto Macone
Separations 2025, 12(7), 183; https://doi.org/10.3390/separations12070183 - 9 Jul 2025
Viewed by 293
Abstract
Gallic acid, a major phenolic compound in wine, significantly influences its sensory profile and health-related properties, making its accurate measurement essential for both enological and nutritional studies. In this context, a derivatization protocol for gallic acid using ethyl chloroformate (ECF) was developed and [...] Read more.
Gallic acid, a major phenolic compound in wine, significantly influences its sensory profile and health-related properties, making its accurate measurement essential for both enological and nutritional studies. In this context, a derivatization protocol for gallic acid using ethyl chloroformate (ECF) was developed and optimized for GC-MS analysis, with experimental conditions refined through a Box–Behnken Design (BBD). The BBD systematically investigated the effects of three critical reagent volumes: ethyl chloroformate, pyridine, and ethanol. This approach elucidated complex interactions and quadratic effects, leading to a predictive second-order polynomial model and identifying the optimal derivatization conditions for maximum yield (137 µL of ethyl chloroformate, 51 µL of pyridine, and 161 µL of ethanol per 150 µL of wine). The BBD-optimized GC-MS method was validated and successfully applied to quantify gallic acid in diverse commercial wine samples (white, red, conventional, natural). A key finding was the method’s wide dynamic range, enabling accurate quantification from 5 up to over 600 µg/mL without sample dilution. This work represents, to our knowledge, the first application of a BBD for optimizing the ethyl chloroformate derivatization of gallic acid, providing a robust, efficient, and widely applicable analytical tool for routine quality control and enological research. Full article
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22 pages, 1203 KiB  
Review
Impact of Use of Ultrasound-Assisted Extraction on the Quality of Brazil Nut Oil (Bertholletia excelsa HBK)
by Orquidea Vasconcelos dos Santos, Sara Camila Vidal Freires, Helen Cristina de Oliveira Palheta and Paulo Henrique de Melo Ferreira
Separations 2025, 12(7), 182; https://doi.org/10.3390/separations12070182 - 8 Jul 2025
Viewed by 380
Abstract
The quality of materials extracted from plant sources, such as oilseeds, is significantly affected by the extraction techniques employed. Thermo-photosensitive bioactive compounds are especially susceptible, often resulting in a loss of functional properties during conventional processing. In this context, studies involving unconventional or [...] Read more.
The quality of materials extracted from plant sources, such as oilseeds, is significantly affected by the extraction techniques employed. Thermo-photosensitive bioactive compounds are especially susceptible, often resulting in a loss of functional properties during conventional processing. In this context, studies involving unconventional or “innovative” extraction methods have emerged as a strategic approach to preserve the quality of the extracted material (whether by-product or biomass) by aligning with the core principles of green chemistry and the expansion of sustainable production chains. This approach promotes both raw material integrity and the protection of human and environmental health. These efforts contribute to a virtuous cycle of technological innovation and environmentally sound practices. This review focuses on how ultrasound-assisted extraction affects the quality of plant-derived materials, particularly Brazil nut oil. The article compiles data published over the last five years (2020–2025), following the PRISMA methodology. Recent studies highlight the synergistic potential of ultrasound as a green technology for isolating Brazil nut oil, offering enhanced nutritional and functional properties. This aligns with the growing demand for healthier food products obtained through sustainable industrial processes and presents opportunities for diverse applications across several industry sectors. Full article
(This article belongs to the Special Issue Extraction and Characterization of Food Components)
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13 pages, 1169 KiB  
Article
The Selective Extraction of Natural Sesquiterpenic Acids in Complex Matrices: A Novel Strategy for Isolating Zizanoic Acid in Vetiver Essential Oil
by Ian Gardel Carvalho Barcellos-Silva, Ananda da Silva Antonio, Mateus Curty Cariello da Silva, Fernanda de Melo Regazio Cariello, Fernando Hallwass, Monica Costa Padilha and Valdir Florencio Veiga-Junior
Separations 2025, 12(6), 163; https://doi.org/10.3390/separations12060163 - 17 Jun 2025
Viewed by 314
Abstract
Essential oils are complex mixtures of apolar components, mainly phenylpropanoids, monoterpenes, and sesquiterpenes. Vetiver (Vetiveria zizanioides (L.) Nash) is a non-endemic grass in several tropical regions, widely used for slope stabilization and erosion control because of its long and deep roots that [...] Read more.
Essential oils are complex mixtures of apolar components, mainly phenylpropanoids, monoterpenes, and sesquiterpenes. Vetiver (Vetiveria zizanioides (L.) Nash) is a non-endemic grass in several tropical regions, widely used for slope stabilization and erosion control because of its long and deep roots that help to bind the soil together, preventing landslides and soil loss. From these roots, vetiver essential oil is obtained, which is extracted and produced worldwide and highly valued for its diverse range of bioactive substances used by the cosmetics and perfume industries. These substances, present in a very complex mixture, are difficult to isolate. Zizanoic acid is a very rare substance in nature and also very interesting because of the biological properties already described. In the present study, zizanoic acid was selectively isolated with 84–87% purity from vetiver commercial essential oils, in which it was present at less than 10%, using KOH-impregnated silica gel column chromatography alone. The experiments were monitored using GC-MS and UHPLC-HRMS, and the isolated substances (zizanoic and valerenic acids) were further determined by NMR experiments. The whole methodology and analytical approach proved to be very efficient for natural product complex mixture analysis and also very selective, allowing for a distinct capacity to recover carboxylic acids from complex biological samples. Full article
(This article belongs to the Special Issue Extraction and Characterization of Food Components)
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27 pages, 3488 KiB  
Review
Current Perspectives on the Extraction, Isolation, and Identification of Fats and Fatty Acids Using Conventional and Green Methods
by Ytaiara Lima-Pereira, Esther Maria Oliveira de Souza, David Silva dos Reis, Ian Gardel Carvalho Barcellos-Silva, Karine Sayuri Lima Miki, Valdir F. Veiga-Júnior and Barbara Elisabeth Teixeira-Costa
Separations 2025, 12(6), 160; https://doi.org/10.3390/separations12060160 - 13 Jun 2025
Viewed by 843
Abstract
The global demand for oils and lipids, particularly those derived from vegetable sources with high polyunsaturated fatty acid content, has posed significant challenges for the food industry. This trend is largely driven by growing consumer awareness of health and nutrition. To meet this [...] Read more.
The global demand for oils and lipids, particularly those derived from vegetable sources with high polyunsaturated fatty acid content, has posed significant challenges for the food industry. This trend is largely driven by growing consumer awareness of health and nutrition. To meet this demand, it is essential to not only identify richer sources of lipids but also develop efficient, sustainable, and environmentally friendly methods for their extraction, isolation, and characterization. In this context, the present work provides a comprehensive review of current perspectives on the extraction, isolation, and identification of lipids and fatty acids, comparing conventional and green methodologies for food applications. Ideally, analytical and processing methodologies for obtaining food-grade materials should prioritize low energy consumption, minimal or no use of hazardous substances, and the generation of non-polluting residues, thereby safeguarding both human health and the environment. In recent years, green extraction techniques have emerged as promising alternatives to conventional methods, offering partial or complete replacements, such as ultrasound-assisted extraction, microwave-assisted extraction, supercritical and subcritical fluid extraction, and others. However, significant advancements are still required to fully address these concerns. Techniques such as chromatography and spectrometry play pivotal roles in the isolation and identification process, especially gas chromatography coupled with mass spectrometry or with flame ionization detectors; while separating individual fatty acids based on their chain length and degree of unsaturation, reversed-phase high-performance liquid chromatography (HPLC) is quite a helpful approach. Furthermore, the isolation and structural elucidation of fatty acids are critical steps in ensuring the nutritional quality and commercial viability of lipid products. Full article
(This article belongs to the Special Issue Extraction and Characterization of Food Components)
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14 pages, 1954 KiB  
Article
Sunflower Seed Oil Enriched with Compounds from the Turmeric Rhizome: Extraction, Characterization and Cell Viability
by Késia Corsato de Oliveira Segantini, Oscar de Oliveira Santos Junior, Vitor Augusto Dos Santos Garcia, Djéssica Tatiane Raspe and Camila da Silva
Separations 2025, 12(5), 121; https://doi.org/10.3390/separations12050121 - 11 May 2025
Cited by 1 | Viewed by 534
Abstract
The present work aimed to obtain and characterize sunflower seed oil (SO) enriched with compounds from turmeric rhizome (TR). For this purpose, the enriched oil was obtained from two strategies: extraction of the compounds from TR using SO as solvent (ESO) and simultaneous [...] Read more.
The present work aimed to obtain and characterize sunflower seed oil (SO) enriched with compounds from turmeric rhizome (TR). For this purpose, the enriched oil was obtained from two strategies: extraction of the compounds from TR using SO as solvent (ESO) and simultaneous extraction of SO and TR compounds using ethyl acetate as solvent (ESOS). In these strategies, the effect of time (15 and 30 min) and temperature (60 and 70 °C) on the enrichment in relation to the curcuminoids content was determined. Evaluation of phytochemicals such as total phenolic compounds (TPCs), phenolic compound profile and fatty-acid profile and bioactivity by antioxidant potential (AP) was carriedoutin the enriched oils and in the SO;mean while, oxidative stability and cytotoxicity were evaluated using HaCaT (human immortalized keratinocyte) cells. From the results obtained, higher contents of curcuminoids (510 mg/100 g oil) were observed in the oil obtained from simultaneous extraction (ESOS) in a shorter time and lower temperature (15 min and 60 °C), and similar behavior was found for the content of phenolic compounds and antioxidant potential. The profile of phenolic compounds revealed the presence of phenolic acids, curcuminoids and terpenes in the composition of the enriched oils, which increased oxidative stability. The oils obtained did not show any cytotoxic effect against the cells tested, confirmed by the high survival rate (>88%) after 48 h of exposure. Full article
(This article belongs to the Special Issue Application of Sustainable Separation Techniques in Food Processing)
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17 pages, 2019 KiB  
Article
Free Fatty Acid Determination in Alcoholic and Non-Alcoholic Beers via Liquid Chromatography–High-Resolution Mass Spectrometry Analysis
by Christiana Mantzourani and Maroula G. Kokotou
Separations 2025, 12(5), 114; https://doi.org/10.3390/separations12050114 - 1 May 2025
Viewed by 2201
Abstract
In recent years, non-alcoholic beers have been gaining popularity. Among the various components that affect the flavor and sensory characteristics of beers, free fatty acids (FFAs) are minor components. However, due to their involvement in beer quality, fast and simple methods for analyzing [...] Read more.
In recent years, non-alcoholic beers have been gaining popularity. Among the various components that affect the flavor and sensory characteristics of beers, free fatty acids (FFAs) are minor components. However, due to their involvement in beer quality, fast and simple methods for analyzing FFAs in beers are of importance. In this work, we present a liquid chromatography–high-resolution mass spectrometry (LC-HRMS) method for the rapid determination of FFAs in beers, avoiding a tedious sample preparation and derivatization and allowing the simultaneous study of a large set of FAs, including medium-chain, long-chain, saturated, monounsaturated and polyunsaturated FAs. The method was applied in the analysis of twelve non-alcoholic and nine alcoholic beer samples from the local market, permitting the comparison of their FFA profiling. Among the 37 FAs studied, 29 were quantified, and palmitic, stearic, oleic and myristic acids were identified as the predominant FAs in both alcoholic and non-alcoholic beers. The majority of the predominant long-chain FAs, including palmitic, stearic and myristic acids, were found in decreased amounts in non-alcoholic beers, compared to the alcoholic ones, with the marked exception of oleic acid, which was increased in non-alcoholic beers. Among the medium-chain FAs, octanoic acid was found at lower concentrations in non-alcoholic beers, comparing to regular beers, while lauric acid was slightly increased. Principal component analysis (PCA) suggested the correlation of FFAs with the type of beer (alcoholic or non-alcoholic beer). Full article
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14 pages, 680 KiB  
Article
Ultrasound-Assisted Extraction of Phenolic Compounds and Flavonoids from Banana Inflorescence and Characterization of Its Fibrous Residue
by Fábio Dias Bertoco Júnior, Érica Marusa Pergo Coelho, Mirian Cristina Feiten and Beatriz Cervejeira Bolanho Barros
Separations 2025, 12(5), 109; https://doi.org/10.3390/separations12050109 - 25 Apr 2025
Viewed by 867
Abstract
The banana inflorescence (BI) is a rich source of antioxidants and dietary fiber, making it a valuable by-product of banana harvesting. This study aimed to maximize the ultrasound-assisted extraction (UAE) of antioxidant compounds from BI and analyze the residue’s composition and functional properties. [...] Read more.
The banana inflorescence (BI) is a rich source of antioxidants and dietary fiber, making it a valuable by-product of banana harvesting. This study aimed to maximize the ultrasound-assisted extraction (UAE) of antioxidant compounds from BI and analyze the residue’s composition and functional properties. The Box–Behnken Design was applied to test different ultrasound powers, temperatures, and sample-to-solvent ratios on the total phenolic content (TPC) and total flavonoid content (TFC). The UAE conducted at 350 W, 55 °C, 1:30 (g/mL) ratio for 30 min resulted in the highest TPC (1637.12 mg/100 g) and TFC (22.97 mg/100 g). Isovanillin, caffeine, naringin, sinapaldehyde, nicotinic acid, quinic acid, malic acid, and fumaric acids were reported for the first time for BI. The extract obtained by UAE showed a higher content of these compounds and higher antioxidant activity than that obtained through conventional extraction (orbital shaking). The residue obtained after UAE presented dietary fiber as the main component (71.91 g/100 g) and a higher oil absorption index (5.78 g/g) than untreated BI. Therefore, BI is a source of bioactive compounds, and both the extract and residue can be used in the pharmaceutical, food, and cosmetic industries, enabling the productive sector to move closer to the circular economy. Full article
(This article belongs to the Special Issue Application of Sustainable Separation Techniques in Food Processing)
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14 pages, 1759 KiB  
Article
Electrochemical Precipitation of Struvite from Wastewater: A Sustainable Approach for Nitrogen Recovery
by Rúbia Mores, Anildo Cunha Junior, Fabiane Goldschmidt Antes, Marco Di Luccio, Carolina E. Demaman Oro, Marcus V. Tres, Clarice Steffens, Juliana Steffens, Airton Kunz and Rogério Marcos Dallago
Separations 2025, 12(5), 108; https://doi.org/10.3390/separations12050108 - 25 Apr 2025
Viewed by 843
Abstract
This study evaluates the feasibility of nitrogen recovery from wastewater via electrochemical methods as an alternative nutrient source for agricultural applications. Ammonium nitrogen (NH4+-N) and phosphate (PO43−-P) contamination poses significant environmental risks and challenges water resource management [...] Read more.
This study evaluates the feasibility of nitrogen recovery from wastewater via electrochemical methods as an alternative nutrient source for agricultural applications. Ammonium nitrogen (NH4+-N) and phosphate (PO43−-P) contamination poses significant environmental risks and challenges water resource management globally. The electrochemical precipitation of struvite (MgNH4PO4·6H2O) offers a promising solution for nutrient recovery, with potential applications as a slow-release fertilizer. Experimental results demonstrate that increased current density (from 2.5 to 7.5 mA/cm2) and reduced electrode distance (1 cm) significantly enhance NH4+ and PO43− consumption and struvite precipitation. Increasing the amperage from 2.5 to 7.5 mA·cm−2 at a 1 cm electrode distance raised the ammoniacal nitrogen incorporation from 1.59 to 5.34 g/100 g, signifying greater struvite production. The Mg and P concentrations were 15.44 and 12.60 g/100 g, respectively, for this higher amperage, although lower than the concentrations seen with 2.5 mA·cm−2 (22.16 and 14.52 g/100 g). The majority of Mg (60%) and P (93.6%) were, however, incorporated within struvite. Additionally, this study reveals that Mg is primarily incorporated as struvite when using higher current densities, while lower current densities yield greater Mg incorporation in non-struvite forms, such as magnesium carbonate. Findings suggest that optimizing current density and electrode distance can improve nitrogen and phosphorus recovery efficiencies, making electrochemical struvite production a viable, sustainable approach for nutrient recycling. This method not only reduces dependence on synthetic fertilizers but also supports sustainable agricultural practices by transforming wastewater contaminants into valuable resources. Full article
(This article belongs to the Special Issue Application of Sustainable Separation Techniques in Food Processing)
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10 pages, 1639 KiB  
Article
Detection of Honey Adulteration by Liquid Chromatography—High-Resolution Mass Spectrometry: Results from an EU Coordinated Action
by Viviana Paiano, Andreas Breidbach, Carolin Lörchner, Tereza Ždiniaková, Olivier De Rudder, Alain Maquet, Lourdes Alvarellos and Franz Ulberth
Separations 2025, 12(2), 47; https://doi.org/10.3390/separations12020047 - 13 Feb 2025
Cited by 2 | Viewed by 3733
Abstract
Honey, a sweet and nutritious food produced by honeybees, is extensively consumed by humans due to its potential health benefits. Unfortunately, the adulteration of honey with inexpensive sugar syrups is a prevalent issue. Verifying the authenticity of honey is crucial for maintaining its [...] Read more.
Honey, a sweet and nutritious food produced by honeybees, is extensively consumed by humans due to its potential health benefits. Unfortunately, the adulteration of honey with inexpensive sugar syrups is a prevalent issue. Verifying the authenticity of honey is crucial for maintaining its quality and safety standards. The aim of this study was to identify the illicit addition of sugar syrups to honey imported into the European Union (EU). The European Commission’s Joint Research Centre (JRC) has employed different analytical approaches to detect several markers of adulteration in honey; however, this paper mainly focuses on the use of Liquid Chromatography–High-Resolution Mass Spectrometry (LC-HRMS). Two qualitative methods were developed to detect mannose (Man), difructose anhydride III (DFA III), 2-acetylfuran-3-glucopyranoside (AFGP), and oligo-/polysaccharides with degrees of polymerization (DPs) of 6 to 11. Out of the 320 honey samples provided by the authorities of the participating EU Member States, 147 (46%) were suspicious for non-compliance with the EU Honey Directive 2001/110/EC, mostly due to the presence of mannose and oligo-/polysaccharides. As a result, the development and standardization of sophisticated and universally recognized testing procedures will increase the capability of official control laboratories to detect honey adulteration and will serve as a powerful preventive measure against fraudulent practices in the global honey market. Full article
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11 pages, 1947 KiB  
Article
Exploring Chicken Feathers as a Cost-Effective Adsorbent for Aqueous Dye Removal
by Marcela Caovilla, Carolina E. Demaman Oro, Rúbia Mores, Luciana D. Venquiaruto, Marcelo L. Mignoni, Marco Di Luccio, Helen Treichel, Rogério Marcos Dallago and Marcus V. Tres
Separations 2025, 12(2), 39; https://doi.org/10.3390/separations12020039 - 6 Feb 2025
Viewed by 879
Abstract
This study explored the use of chicken feathers, a low-cost and abundant agricultural byproduct, as a sorbent for the removal of reactive yellow dye from aqueous solutions. The dual potential of feathers as both adsorbents and sorbents, attributed to their keratin-rich structure, was [...] Read more.
This study explored the use of chicken feathers, a low-cost and abundant agricultural byproduct, as a sorbent for the removal of reactive yellow dye from aqueous solutions. The dual potential of feathers as both adsorbents and sorbents, attributed to their keratin-rich structure, was utilized to investigate their effectiveness in dye removal. Feathers, activated with 1.0 mol/L HCl, exhibited a maximum adsorption capacity at 70 °C and pH 5.5, as determined from Langmuir isotherm modeling. A 22 central composite rotatable design revealed that temperature and pH significantly influence the adsorption efficiency, with higher temperatures favoring the process. Kinetic studies demonstrated pseudo-first-order behavior, with rapid initial adsorption reaching equilibrium within 120 min. Thermodynamic analysis confirmed the endothermic nature of the process (ΔH° = 28.04 kJ mol−1), a positive entropy change (ΔS° = 66.62 J/mol·K), and a reduction in Gibbs free energy (ΔG°) with increasing temperature, suggesting enhanced feasibility at elevated temperatures. This research highlights the potential of utilizing poultry industry residues as sustainable and efficient sorbents for environmental remediation, contributing to waste valorization and eco-friendly wastewater treatment solutions. Full article
(This article belongs to the Special Issue Application of Sustainable Separation Techniques in Food Processing)
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15 pages, 2867 KiB  
Article
Rapid Classification of Unroasted Green Coffee Beans and Spices Based on the Tentative Determination of Volatile Compounds by Solid-Phase Dynamic Extraction (SPDE) and Gas Chromatography–Mass Spectrometry (GC–MS) with Supervised Learning
by Dimitrios G. Lazaridis, Evelyna K. Kokkosi, Emmanouela N. Mylonaki, Vassilios K. Karabagias, Nikolaos D. Andritsos and Ioannis K. Karabagias
Separations 2024, 11(12), 351; https://doi.org/10.3390/separations11120351 - 14 Dec 2024
Cited by 2 | Viewed by 1227
Abstract
The present study comprises the second part of our previous work that dealt mainly with the phytochemical and physicochemical characterization of commercial unroasted green coffee beans, clove, cinnamon–clove and nutmeg ethanolic extracts of grape origin. In the present study, we focused on producing [...] Read more.
The present study comprises the second part of our previous work that dealt mainly with the phytochemical and physicochemical characterization of commercial unroasted green coffee beans, clove, cinnamon–clove and nutmeg ethanolic extracts of grape origin. In the present study, we focused on producing a discriminating model concerning commercial unroasted green coffee beans, clove, cinnamon, cinnamon and clove mixture (1:1, w/w), and nutmeg fine powders based on multivariate analysis of variance and supervised learning from tentative data of volatile compounds analysis, carried out with solid phase dynamic extraction in combination with gas chromatography–mass spectrometry. Results showed that 7 volatile compounds, i.e., ethylene, methanol, 3-methylpentane, ethyl acetate, 9-hexadecen-1-ol, toluene, and methyl acetate, could differentiate the investigated samples resulting in a 100% classification rate using the cross-validation method of linear discriminant analysis. Results were further confirmed using partial least squares regression analysis. The study contributes to the typification of commercial unroasted green coffee beans, cinnamon, clove, cinnamon and clove mixture, and nutmeg, based on selected volatile compounds. In addition, the study provides further support to the literature by means of a possible substitution of these products in rapid analysis tests, given the statistical models developed. Full article
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18 pages, 2924 KiB  
Article
Comparison and Optimization of Three Extraction Methods for Epimedium polysaccharides
by Cheng Liu, Fangyuan Gong, Yijia Chen, Zhengwei Xiong, Cun Wang, Jiepei Li and Jin Guo
Separations 2024, 11(10), 296; https://doi.org/10.3390/separations11100296 - 14 Oct 2024
Cited by 1 | Viewed by 1326
Abstract
Epimedium is used in traditional Chinese medicine. Epimedium polysaccharides have a variety of physiological properties. This study compared three different processes for the extraction of polysaccharides from Epimedium spp., including ultrasonic, aqueous enzymatic, and microwave extraction, to optimize the extraction conditions and determine [...] Read more.
Epimedium is used in traditional Chinese medicine. Epimedium polysaccharides have a variety of physiological properties. This study compared three different processes for the extraction of polysaccharides from Epimedium spp., including ultrasonic, aqueous enzymatic, and microwave extraction, to optimize the extraction conditions and determine the optimal extraction method. The optimal parameters for each method were analyzed. The results showed that the optimal process for ultrasonic extraction was an ultrasonic power of 250 W, an extraction time of 60 min, a temperature of 50 °C, and a solid–liquid ratio of 1:35. The optimal conditions for the aqueous enzymatic method were a papain concentration of 70 U/mL, extraction time of 70 min, a temperature of 50 °C, and a material-to-liquid ratio of 1:30, while those for microwave extraction were a microwave power of 650 W, an extraction time of 50 min, a temperature of 40 °C, and a material-to-liquid ratio of 1:25. The polysaccharide yields were 4.85%, 4.72%, and 3.98% for the three methods, respectively, indicating that ultrasonic extraction resulted in the highest yield of polysaccharides from Epimedium brevicornum. After purification with DEAE-cellulose, the polysaccharide yields were 4.13%, 3.67%, and 3.12%, respectively. A comprehensive comparison demonstrated the superiority of the ultrasonic extraction method in terms of both extraction yield and purification efficiency. Characterization of the extracted Epimedium polysaccharides showed the presence of five monosaccharides, i.e., glucose, galactose, mannose, galacturonic acid, and rhamnose, and a number average molecular weight Mn of 1.65 × 105 Da and weight average molecular weight Mw of 6.61 × 105 Da. These results provide a scientific basis for the in-depth study and application of Epimedium polysaccharides. Full article
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