Article
Biochemical Research Methods
Sergio M. Vilas-Boas, Isabella W. Cordova, Kiki A. Kurnia, Heloisa H. S. Almeida, Priscilla S. Gaschi, Joao A. P. Coutinho, Simao P. Pinho, Olga Ferreira
Summary: Countercurrent and centrifugal partition chromatography are techniques for separating compounds from natural extracts, with the selection of the biphasic solvent system being a key design parameter. COSMO-RS and NRTL-SAC models were used to estimate partition coefficients of phenolic compounds in different solvent systems, with the NRTL-SAC model showing higher reliability.
JOURNAL OF CHROMATOGRAPHY A
(2022)
Article
Biochemical Research Methods
Jean-Baptiste Chagnoleau, Ines L. D. Ryan, Ryan Khedher, Joao AP Coutinho, Thomas Michel, Xavier Fernandez, Nicolas Papaiconomou
Summary: A study was conducted on ternary biphasic systems composed of heptane, 1-butanol or ethyl acetate, and type III or type V deep eutectic solvents based on levulinic acid and choline chloride or thymol. The binodal curves, densities, and phase compositions of the equilibrium phases were determined for seven systems. The partition coefficients of six natural compounds were measured in these systems. Based on the results, a system composed of heptane, 1-butanol, and the deep eutectic solvent choline chloride:levulinic acid at a molar ratio of 1:3 was selected for centrifugal partition chromatography and showed good separation of apigenin, coumarin, beta-ionone, and alpha-tocopherol.
JOURNAL OF CHROMATOGRAPHY A
(2023)
Article
Biochemical Research Methods
Tim Hammerschick, Walter Vetter
Summary: Centrifugal partition chromatography (CPC) and countercurrent chromatography (CCC) are two preparative techniques used for the isolation and purification of natural products. This study successfully combined the advantages of both techniques by directly linking CPC and CCC, and demonstrated the effectiveness of the hybrid system.
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
(2022)
Article
Engineering, Chemical
Ariane A. Oshiro, Alexandre M. S. Jorge, Valeria C. Santos-Ebinuma, Jorge F. B. Pereira
Summary: This study proposes an aqueous two-phase system (ATPS) composed of ethanol and dipotassium hydrogen phosphate for Centrifugal Partition Chromatography (CPC). Compared to polymer-based ATPS, the Ethanol/K2HPO4 system overcomes hydrodynamic drawbacks and demonstrates advantages such as short settling time, high interfacial tension, significant density differences, and low viscosity. CPC experiments show that controlling the operating parameters can achieve stable conditions and successful separation of biomolecules using the ethanol/salt ATPS.
SEPARATION AND PURIFICATION TECHNOLOGY
(2024)
Article
Chemistry, Physical
Alvaro Silva Lima, Bruno Sales de Oliveira, Selesa Vanessa Shabudin, Mafalda Almeida, Mara Guadalupe Freire, Katharina Bica
Summary: This work aimed to integrate the extraction and purification of anthocyanins from grape pomace using ATPS and scaled-up CPC, with protic ionic liquids as the common solvent. Different operational conditions led to varied purification factors, with ATPS and CPC achieving significant purification of anthocyanins. The choice of optimal operational conditions depends on the specific application of anthocyanins.
JOURNAL OF MOLECULAR LIQUIDS
(2021)
Article
Engineering, Chemical
Mafalda R. Almeida, Filipe Ferreira, Pedro Domingues, Joao A. P. Coutinho, Mara G. Freire
Summary: This study successfully developed a method to purify IgY from egg yolk, combining water-soluble protein fraction and aqueous biphasic systems, followed by centrifugal partition chromatography for purification. The operating conditions of CPC were optimized to obtain IgY with high purity.
SEPARATION AND PURIFICATION TECHNOLOGY
(2022)
Article
Chemistry, Multidisciplinary
Ines L. D. Rocha, Andre M. da Costa Lopes, Sonia P. M. Ventura, Joao A. P. Coutinho
Summary: This study utilized a PEG/NaPA ABS system assisted CPC for the separation of lignin-derived monomers, showing that ILs are more suitable than inorganic salts for compound partition in CPC. Alkaline conditions were found to enhance the partition of vanillic acid, and pH was identified as a crucial factor in the separation of lignin monomer compounds.
ACS SUSTAINABLE CHEMISTRY & ENGINEERING
(2022)
Article
Chemistry, Applied
Angela L. Alarcon, Laura M. Palacios, Coralia Osorio, Paulo Cesar Narvaez, Francisco J. Heredia, Alvaro Orjuela, Dolores Hernanz
Summary: The study found that non-centrifugal cane sugar samples obtained by traditional moulding and granulation, as well as through a novel spray-drying powdering process, have different sugar and phenolic profiles, flavonoid content, and color parameters. The thermal treatment in the production of granulated products led to darker colors and changes in phenol and flavonoid contents, while spray drying produced clearer products with slightly lower phenol and flavonoid contents.
Article
Chemistry, Analytical
Fabian Hammerle, Michael Zwerger, Anja Hoeck, Markus Ganzera, Ursula Peintner, Bianka Siewert
Summary: Recently, it has been discovered that certain fungal pigments have significant photoactivity, making them promising candidates for treating microbial infections or malignant diseases. In this study, a separation method for fungal anthraquinones was developed using centrifugal partition chromatography. The method was successfully applied to purify multiple pigments from fungal extracts.
JOURNAL OF SEPARATION SCIENCE
(2022)
Article
Biochemical Research Methods
Thomas Michel, Celestine Loyet, Romain Boulho, Magalie Eveno, Gregoire Audo
Summary: Centrifugal partition chromatography (CPC) is a liquid-liquid chromatography technique that separates compounds by continuous partition between two immiscible phases. The main objective of this study was to replace traditional solvents with sustainable alternatives in CPC, leading to the isolation of natural products with high purity.
PHYTOCHEMICAL ANALYSIS
(2023)
Article
Biotechnology & Applied Microbiology
Hyun-Soo Kim, Ilekuttige Priyan Shanura Fernando, Seung-Hong Lee, Seok-Chun Ko, Min Cheol Kang, Ginnae Ahn, Jun-Geon Je, K. K. A. Sanjeewa, Jung-Rae Rho, Hee Jae Shin, WonWoo Lee, Dae-Sung Lee, You-Jin Jeon
Summary: This study focused on developing methods for sustainable use of Sargassum horneri biomass. Three bioactive compounds were isolated from methanol extracts of S. horneri, showing potential anti-inflammatory properties. Further research could lead to the development of these compounds as cosmetics and functional food materials.
ALGAL RESEARCH-BIOMASS BIOFUELS AND BIOPRODUCTS
(2021)
Article
Biotechnology & Applied Microbiology
Anne Pajot, Sebastien Chollet, Elodie Nicolau, Luc Marchal
Summary: This study aims to optimize the recovery and purity of fucoxanthin from Tisochrysis lutea using the CPC technique. CPC provides fast and room temperature extraction without degradation. By optimizing the solvent composition and operating conditions, nine fractions with 100% purity and 92% recovery yield were obtained.
ALGAL RESEARCH-BIOMASS BIOFUELS AND BIOPRODUCTS
(2023)
Article
Engineering, Chemical
Bruna P. Soares, Joao H. P. M. Santos, Margarida Martins, Mafalda R. Almeida, Nathalia Santos, Mara G. Freire, Valeria C. Santos-Ebinuma, Joao A. P. Coutinho, Jorge F. B. Pereira, Sonia P. M. Ventura
Summary: This study investigated the continuous purification of EGFP using ABS, with an initial screening conducted by changing the electrolyte content in the ABS to find the optimal conditions. The results showed a high purification rate (89.93%) and recovery yield (82.3%), indicating the potential of FCPC for the continuous purification of EGFP.
SEPARATION AND PURIFICATION TECHNOLOGY
(2021)
Article
Biochemistry & Molecular Biology
Magdalena Maciejewska-Turska, Lukasz Pecio, Grazyna Zgorka
Summary: Pueraria lobata is a legume plant native to Southeast Asia, widely used in traditional medicine. This study developed an original preparative method to efficiently isolate hydrophilic daidzein C-glycosides, including mirificin, from kudzu roots. The isolated mirificin showed a purity of 63% and exhibited significant anti-biodegenerative effects.
Article
Biochemistry & Molecular Biology
Magdalena Bartnik
Summary: Pure methoxyfuranocoumarins were successfully isolated from fruits of Peucedanum tauricum MB. using counter-current chromatography. The optimized biphasic solvent system and validated HPLC-DAD-ESI-MS method were used for the isolation, identification, and quantification of the compounds. The obtained high purity of the plant metabolites makes them suitable for pharmacological or biological studies.
Article
Energy & Fuels
Mafalda R. Almeida, Rita A. M. Barros, Matheus M. Pereira, Daniel Castro, Joaquim L. Faria, Mara G. Freire, Claudia G. Silva, Ana P. M. Tavares
Summary: Nanomaterials, especially carbon-based nanomaterials, have been widely used in various biomedical applications. In this study, a process intensification approach for attaching immunoglobulin G (IgG) to multi-walled carbon nanotubes (MWCNTs) was proposed and evaluated. The effect of different parameters on the IgG attachment yield was investigated, and it was found that dilution of rabbit serum increased the IgG yield while decreasing other protein attachment. The orientation of IgG on the MWCNTs surface was determined to be end-on, which suggests that this attachment strategy could be effective for antigen recognition and biomedical applications.
CHEMICAL ENGINEERING AND PROCESSING-PROCESS INTENSIFICATION
(2023)
Article
Chemistry, Multidisciplinary
Carlos M. N. Mendonc, Nathalia V. Verissimo, Wellison A. . Pereira, Paula M. Cunha, Michele Vitolo, Attilio Converti, Kiki Adi Kurnia, Fernando Segato, Pamela O. S. de Azevedo, Mara G. Freire, Koen Venema, Joao H. P. M. Santos, Ricardo P. S. Oliveira
Summary: Aqueous biphasic systems (ABSs) based on sodium polyacrylate (NaPA), ethylene oxide/propylene oxide (EO/PO) polymers, and (EO)x-(PO)y-(EO)x triblock copolymers were prepared and applied for continuous fructooligosaccharide (FOS) production and separation. The hydrophilicity/hydrophobicity balance of EO/PO had a significant effect on ABS formation. Different carbohydrates and levansucrase showed different partition behavior in these ABSs. By selecting the appropriate ABS composition, high yields of FOS and selective partitioning could be achieved. COSMO-RS suggested that ABS formation was due to competition between NaPA and polymers/copolymers to form hydrogen bonds with water molecules.
ACS SUSTAINABLE CHEMISTRY & ENGINEERING
(2023)
Article
Engineering, Chemical
Sergio M. Vilas-Boas, Isabella W. Cordova, Dinis O. Abranches, Joao A. . P. Coutinho, Olga Ferreira, Simao P. Pinho
Summary: In this study, the Abraham and NRTL-SAC semi-predictive models were used to represent the solubility of different solutes in water and organic solvents. The models were calibrated using measured and literature data, and their predictive capabilities were tested on independent solvents. The results showed that NRTL-SAC performed better in the correlation/prediction approach, while COSMO-RS could produce satisfactory predictions even without experimental data.
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
(2023)
Article
Engineering, Chemical
Sergio M. Vilas-Boas, Aline Zambom Coelho, Monia A. R. Martins, Joao A. P. Coutinho, Olga Ferreira, Simao P. Pinho
Summary: In this study, the potential use of ionic liquids (ILs) and their mixtures as separation agents in the fractionation of essential oils was investigated. Experimental and modeling approaches showed that chloride-based ILs are effective in fractionating essential oils containing hydrogen-bond donor monoterpenoids.
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
(2023)
Article
Engineering, Chemical
Goncalo M. C. Silva, German Perez-Sanchez, Diego A. Pantano, Sophie Loehle, Joao A. P. Coutinho
Summary: In this study, the SAFT-gamma-Mie equation of state was used to develop coarse-grained molecular models for describing micellization phenomena in a top-down approach. Polyethylene oxide (PEO)/polypropylene oxide (PPO) triblock copolymers in aqueous solutions were selected as the case study. The model was successfully fitted to reproduce the thermophysical properties and liquid-liquid phase diagrams of PEO/PPO oligomers and their mixtures with water. Molecular dynamics simulations showed the formation of spherical micelles with star-shaped or flower-shaped morphology at low concentrations, and the formation of larger micelles or aggregates at higher concentrations.
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
(2023)
Article
Biochemistry & Molecular Biology
Ignacio Sanchez-Moguel, Tales A. Costa-Silva, Omar S. Pillaca-Pullo, Juan Carlos Flores-Santos, Rominne Karla Barros Freire, Gustavo Carretero, Julia da Luz Bueno, David I. Camacho-Cordova, Joao H. P. M. Santos, Lara Duraes Sette, Adalberto Pessoa-
Summary: Microorganisms from extreme environments, like the Antarctic ecosystems, have the potential to produce enzymes with unique characteristics. In this study, a yeast species called Leucosporidium scottii from Admiralty Bay in Antarctica was found to produce L-asparaginase (ASNase) with low glutaminase activity. The purified ASNase showed high activity at a temperature of 55 degrees C and a pH of 7.5, making it suitable for potential applications.
PROCESS BIOCHEMISTRY
(2023)
Article
Pharmacology & Pharmacy
Sonia N. Pedro, Ana T. P. C. Gomes, Carla Vilela, Carla Vitorino, Rosa Fernandes, Adelaide Almeida, Maria Helena Amaral, Mara G. Freire, Armando J. D. Silvestre, Carmen S. R. Freire
Summary: A new type of microemulsion based on deep eutectic solvent (DES) has been developed to improve the efficacy of antibiotics in ocular infections. By using betaine-based DES aqueous solutions, the water solubility of the antibiotic chloramphenicol can be increased up to 140-fold. These DES solutions are applied as water phases in stable water-in-oil-in-water (w/o/w) microemulsions, achieving sustained-release and higher permeation through the cornea. Compared to commercialized eye drops, these microemulsions show higher antimicrobial activity and faster action against methicillin-resistant Staphylococcus aureus (MRSA) infections.
ADVANCED THERAPEUTICS
(2023)
Article
Engineering, Chemical
Thomas Brouwer, Emanuel A. Crespo, Antoon ten Kate, Joao A. P. Coutinho, Sascha R. A. Kersten, Gerrald Bargeman, Boelo Schuur
Summary: This study systematically assessed the feasibility of determining vapor-liquid equilibrium (VLE) data based on excess molar enthalpy (h(E)) results. Twelve cubic Equation of State (cEoS) models combined with eight mixing rules and the Perturbed Chain Statistical Associating Fluid Theory (PC-SAFT) were evaluated. The results showed that the developed h(E)-cEoS-VLE methodology can accurately predict VLE data for systems with unavailable binary interaction parameters, and the h(E)-PC-SAFT-VLE model can accurately predict VLE data for highly nonideal and associating systems.
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
(2023)
Review
Chemistry, Multidisciplinary
Ana R. F. Carreira, Helena Passos, Joao A. P. Coutinho
Summary: The widespread presence of metals in water bodies has driven the development of platforms for their removal and recovery. Biosorption, specifically using algae, has emerged as a sustainable and cost-effective method for metal removal from wastewater. However, there are still gaps in the research, such as limited studies in natural wastewater and a lack of consideration for ion and metal competition. This study explores the application of non-living algae for metal recovery and compares their sorption capacity with other wastewater matrices, as well as evaluating the cost performance compared to commercial and waste-based sorbents.
Article
Chemistry, Multidisciplinary
Cariny Polesca, Amir Al Ghatta, Helena Passos, Joao A. P. Coutinho, Jason P. Hallett, Mara G. Freire
Summary: This study successfully dissolved chicken feathers in an aqueous solution of bio-based ionic liquid, achieving efficient and environmentally friendly keratin recovery. Under optimal recovery conditions, a recovery rate of 93% was achieved, and the ionic liquid showed reusable properties. Techno-economic assessment showed that the produced keratin can be commercialized, with a minimum selling price of $22 per kg and low CO2 emission.
Article
Chemistry, Multidisciplinary
Marguerita E. Rosa, Ana M. Ferreira, Catarina M. S. S. Neves, Mafalda R. Almeida, Rafael Barros, Ana C. Cristovao, Ana C. A. Sousa, Patricia M. Reis, Luis Paulo N. Rebelo, Jose M. S. S. Esperanca, Joao A. P. Coutinho, Mara G. Freire
Summary: Globally, a large amount of root crops, fruits, and vegetables are wasted, including beetroot stems and leaves. A new integrated process has been developed to extract and separate pigments from red beet stems and leaves, contributing to the valorisation of waste biomass.
Article
Chemistry, Physical
Jean -Baptiste Chagnoleau, Nicolas Papaiconomou, Xavier Fernandez, Joao A. P. Coutinho
Summary: This study evaluates the potential of the conductor-like screening model for designing biphasic systems for natural compound separation. The model accurately predicts binodal curves and phases composition and shows excellent agreement with experimental data for partition coefficients of natural compounds. The model is able to capture the influence of changes in system composition on partition coefficients.
JOURNAL OF MOLECULAR LIQUIDS
(2024)
Article
Chemistry, Multidisciplinary
Raul Gonzalez-Martin, Francisca A. e Silva, Maria J. Trujillo-Rodriguez, David Diaz Diaz, Jacob Lorenzo-Morales, Mara G. Freire, Veronica Pino
Summary: This study proposes the use of aqueous biphasic systems as a tool for clean-up, microextraction, and preconcentration of biomarkers in saliva. This innovative approach improves the analysis of saliva in terms of simplicity and environmental friendliness.
Article
Chemistry, Multidisciplinary
Xuemei Liu, Chaonan Cui, Shuoshuo Wei, Jinyu Han, Xinli Zhu, Qingfeng Ge, Hua Wang
Summary: This study presents a new strategy for designing efficient photocatalysts that can convert CO2 into hydrocarbons by utilizing synergistic catalytic sites. The findings provide a solution for the selective photocatalytic reduction of CO2 to CH4.
Article
Chemistry, Multidisciplinary
Chengxian Hu, Dan Wang, Lu Wang, Ying Fu, Zhengyin Du
Summary: A novel one-pot, three-component reaction conducted under electrochemical conditions was studied. The reaction involved 2-aminothiophenols, aldehydes, and malononitrile, using TBABF4 as an electrolyte and CuI as a catalyst. The proposed reaction mechanism suggested that CuI served as an electron relay. This method offers simplified operation, high atom economy, and mild reaction conditions.
Article
Chemistry, Multidisciplinary
Zhi Yang, Yu Chen, Linxi Wan, Yuxiao Li, Dan Chen, Jianlin Tao, Pei Tang, Fen-Er Chen
Summary: A highly enantioselective method for the complete hydrogenation of pyrimidinium salts using Ir/(S,S)-f-Binaphane complex as the catalyst was developed. This method provides easy access to fully saturated chiral hexahydropyrimidines, which are prevalent in many bioactive molecules. The reactions exhibit high yields and enantioselectivities under mild reaction conditions without additives. Successful application of this methodology in a continuous flow fashion further extends its practical utility.
Article
Chemistry, Multidisciplinary
Tina Jeoh, Jennifer Danger Nill, Wujun Zhao, Sankar Raju Narayanasamy, Liang Chen, Hoi-Ying N. Holman
Summary: In this study, the enzymatic hydrolysis of cellulose was investigated using real-time infrared spectromicroscopy. The spatial heterogeneity of cellulose was found to impact the hydrolysis kinetics. Hydration affected cellulose ordering, and Cel7A preferentially removed less extensively hydrogen bonded cellulose.
Article
Chemistry, Multidisciplinary
Tiphaine Richard, Walid Abdallah, Xavier Trivelli, Mathieu Sauthier, Clement Dumont
Summary: An effective method of grafting functionalities onto lignin based on glycerol carbonate has been developed using an efficient nickel-catalysed telomerisation reaction. This method allows lignin to have new reactive functions and reduces the glass transition temperatures of modified lignins, thereby expanding the application range of lignin-based resins.
Article
Chemistry, Multidisciplinary
Jing Qi, Xiyan Wang, Gan Wang, Srinivas Reddy Dubbaka, Patrick ONeill, Hwee Ting Ang, Jie Wu
Summary: This study presents a green and environmentally friendly approach for the synthesis of imides using electrocatalytic oxidation with H2O as the oxygen source. The method eliminates the need for toxic or expensive oxidants and achieves high yields under mild reaction conditions. It shows broad substrate compatibility and potential for industrial applications.
Article
Chemistry, Multidisciplinary
Babasaheb Sopan Gore, Lin-Wei Pan, Jun-Hao Lin, Yi-Chi Luo, Jeh-Jeng Wang
Summary: Here, we report a visible light-promoted intramolecular radical cascade reaction for the construction of fluorenol and naphthalene-fused cyclopropyl carbaldehyde derivatives. This method offers mild reaction conditions, a broad substrate scope, excellent step efficiency, and scalability, without the need for external chemical oxidants. The novelty of this protocol was demonstrated by synthesizing chrysene analogs and performing late-stage functionalizations.
Article
Chemistry, Multidisciplinary
Juho Antti Sirvio, Idamaria Romakkaniemi, Juha Ahola, Svitlana Filonenko, Juha P. Heiskanen, Ari Ammala
Summary: This article discusses the method of using supramolecular interaction between an aromatic hydrogen bond donor and lignin to achieve rapid delignification of softwood at low temperatures.
Article
Chemistry, Multidisciplinary
Yunyan Meng, Chunxiang Pan, Na Liu, Hongjiang Li, Zixiu Liu, Yao Deng, Zixiang Wei, Jianbin Xu, Baomin Fan
Summary: A novel visible light-driven synthesis method for 2,3-diamines has been developed, which has mild conditions, avoids the use of metal reagents, and can synthesize diamines and diols in one pot.
Article
Chemistry, Multidisciplinary
Mingqing Huang, Haiyang Huang, Mengyao You, Xinxin Zhang, Longgen Sun, Chao Chen, Zhichao Mei, Ruchun Yang, Qiang Xiao
Summary: A direct air-oxidized strategy for the synthesis of benzo[b]phosphole oxides was developed in this study. Arylphosphine oxides were transformed into phosphinoyl radicals, which were further combined with various alkynes to achieve the desired products. DFT calculations revealed the mechanism of phosphinoyl radical formation.
Article
Chemistry, Multidisciplinary
Anwei Wang, Jiayin Huang, Chunsheng Zhao, Yu Fan, Junfeng Qian, Qun Chen, Mingyang He, Weiyou Zhou
Summary: This study demonstrates an innovative strategy for the aerobic oxidation of C(sp(3))-H bonds using gamma-valerolactone. By optimizing the reaction conditions and utilizing specific catalysts, efficient oxidation of C(sp(3))-H bonds is achieved with good chemoselectivity in certain cases.
Article
Chemistry, Multidisciplinary
Shun Li, Likai Tong, Zhijian Peng, Bo Zhang, Xiuli Fu
Summary: Sulfide compounds show promise as electrocatalysts for water splitting, but their performance is limited by factors such as limited active sites and hindered substance transport. This study successfully prepared a high-entropy sulfide (ZnCoMnFeAlMg)(9)S-8, which reduced grain size and increased specific surface area, enabling the realization of a dual-functional catalyst with multiple catalytic sites. High entropy also modulated the electronic properties of sulfides, reducing the potential energy barrier for hydrolysis. This research introduces a new approach for functionalizing high entropy nanomaterials and improves the performance of water splitting catalysts.