| 1. |
- Alves, Luis, et al.
(författare)
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Revisiting the dissolution of cellulose in H3PO4(aq) through cryo-TEM, PTssNMR and DWS
- 2021
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Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 252
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Tidskriftsartikel (refereegranskat)abstract
- Cellulose can be dissolved in concentrated acidic aqueous solvents forming extremely viscous solutions, and, in some cases, liquid crystalline phases. In this work, the concentrated phosphoric acid aqueous solvent is revisited implementing a set of advanced techniques, such as cryo-transmission electronic microscopy (cryo-TEM), polarization transfer solid-state nuclear magnetic resonance (PTssNMR), and diffusing wave spectroscopy (DWS). Cryo-TEM images confirm that this solvent system is capable to efficiently dissolve cellulose. No cellulose particles, fibrils, or aggregates are visible. Conversely, PTssNMR revealed a dominant CP signal at 25 °C, characteristic of C-H bond reorientation with correlation time longer than 100 ns and/or order parameter above 0.5, which was ascribed to a transient gel-like network or an anisotropic liquid crystalline phase. Increasing the temperature leads to a gradual transition from CP to INEPT-dominant signal and a loss of birefringence in optical microscopy, suggesting an anisotropic-to-isotropic phase transition. Finally, an excellent agreement between optical microrheology and conventional mechanical rheometry was also obtained.
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| 2. |
- Barea-Sepulveda, Marta, et al.
(författare)
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Total Ion Chromatogram and Total Ion Mass Spectrum as Alternative Tools for Detection and Discrimination (A Review)
- 2022
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Ingår i: CHEMOSENSORS. - : MDPI AG. - 2227-9040. ; 10:11
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Forskningsöversikt (refereegranskat)abstract
- Gas chromatography (GC) and mass spectrometry (MS) are widely used techniques in the analysis of complex mixtures due to their various advantages, such as high selectivity, reproducibility, precision, and sensitivity. However, the data processing is often complex and time-consuming and requires a great deal of experience, which might be a serious drawback in certain areas, such as quality control, or regarding research in the field of medicine or forensic sciences, where time plays a crucial role. For these reasons, some authors have proposed the use of alternative data processing approaches, such as the total ion chromatogram or total mass spectrum, allowing these techniques to be treated as sensors where each retention time or ratio m/z acts as a sensor collecting total intensities. In this way, the main advantages associated with both techniques are maintained, but the outcomes from the analysis can be reached in a faster, simpler, and an almost automated way. In this review, the main features of the GC- and MS-based analysis methodologies and the ways in which to apply them are highlighted. Moreover, their implementation in different fields, such as agri-food, forensics, environmental sciences, or medicine is discussed, highlighting important advantages as well as limitations.
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| 3. |
- Costa, Carolina, et al.
(författare)
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Cellulose-stabilized oil-in-water emulsions : Structural features, microrheology, and stability
- 2021
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Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 252
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Tidskriftsartikel (refereegranskat)abstract
- Cellulose-based oil-in-water (O/W) emulsions were studied by diffusing wave spectroscopy (DWS) regarding the effect of the cellulose concentration and mixing rate on the average droplet size, microrheological features and stability. Furthermore, the microstructure of these emulsions was imaged by cryo-scanning electron microscopy (cryo-SEM). The micrographs showed that cellulose was effectively adsorbed at the oil-water interface, resembling a film-like shell that protected the oil droplets from coalescing. The non-adsorbed cellulose that was observed in the continuous aqueous medium, contributed to the enhancement of the viscosity of the medium, leading to an improvement in the stability of the overall system. Generally, the higher the cellulose concentration and mixing rate, the smaller the emulsion droplets formed, and the higher was their stability. The combination of both techniques, DWS and cryo-SEM, revealed a very appealing and robust methodology for the characterization and design of novel emulsion-based formulations.
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| 4. |
- Costa, Carolina, et al.
(författare)
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Lignin enhances cellulose dissolution in cold alkali
- 2021
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Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 274
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Tidskriftsartikel (refereegranskat)abstract
- Aqueous sodium hydroxide solutions are extensively used as solvents for lignin in kraft pulping. These are also appealing systems for cellulose dissolution due to their inexpensiveness, ease to recycle and low toxicity. Cellulose dissolution occurs in a narrow concentration region and at low temperatures. Dissolution is often incomplete but additives, such as zinc oxide or urea, have been found to significantly improve cellulose dissolution. In this work, lignin was explored as a possible beneficial additive for cellulose dissolution. Lignin was found to improve cellulose dissolution in cold alkali, extending the NaOH concentration range to lower values. The regenerated cellulose material from the NaOH-lignin solvents was found to have a lower crystallinity and crystallite size than the samples prepared in the neat NaOH and NaOH-urea solvents. Beneficial lignin-cellulose interactions in solution state appear to be preserved under coagulation and regeneration, reducing the tendency of crystallization of cellulose.
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| 5. |
- Costa, Carolina, et al.
(författare)
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On the formation and stability of cellulose-based emulsions in alkaline systems : Effect of the solvent quality
- 2022
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Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 286
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Tidskriftsartikel (refereegranskat)abstract
- With amphiphilic properties, cellulose molecules are expected to adsorb at the O/W interface and be capable of stabilizing emulsions. The effect of solvent quality on the formation and stability of cellulose-based O/W emulsions was evaluated in different alkaline systems: NaOH, NaOH-urea and tetrabutylammonium hydroxide (TBAH). The optimal solvency conditions for cellulose adsorption at the O/W interface were found for the alkaline solvent with an intermediate polarity (NaOH-urea), which is in line with the favorable conditions for adsorption of an amphiphilic polymer. A very good solvency (in TBAH) and the interfacial activity of the cation lead to lack of stability because of low cellulose adsorption. However, to achieve long-term stability and prevent oil separation in NaOH-urea systems, further reduction in cellulose's solvency was needed, which was achieved by a change in the pH of the emulsions, inducing the regeneration of cellulose at the surface of the oil droplets (in-situ regeneration).
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| 6. |
- Dahlström, Christina, 1977-, et al.
(författare)
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Regenerated cellulose properties tailored for optimized triboelectric output and the effect of counter-tribolayers
- 2024
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Ingår i: Cellulose. - : Springer Nature. - 0969-0239 .- 1572-882X. ; 31:4, s. 2047-2061
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Tidskriftsartikel (refereegranskat)abstract
- Cellulose has shown great potential in the development of green triboelectric nanogenerators. Particularly, regenerated cellulose (R-cellulose) has shown remarkably high output power density but the structural features and key parameters that explain such superior performance remain unexplored. In this work, wood cellulose fibers were dissolved in a LiOH(aq)-based solvent to produce a series of R-cellulose films. Regeneration in different alcohols (from methanol to n-pentanol) was performed and the films’ structural features and triboelectric performance were assessed. Nonsolvents of increased hydrophobicity led to R-cellulose films with a more pronounced (1–10) diffraction peak. An open-circuit voltage (VOC) of up to ca. 260 V and a short-circuit current (ISC) of up to ca. 150 µA were measured for R-cellulose against polytetrafluoroethylene (as negative counter-layer). However, R-cellulose showed an increased VOC of 175% (from 88.1 V) against polydimethylsiloxane when increasing the alcohol hydrocarbon chain length from methanol to n-pentanol. The corresponding ISC and output power also increased by 76% (from 89.9 µA) and by 382% (from 8.8 W m–2), respectively. The higher R-cellulose hydrophilicity, combined with soft counter-tribolayer that follow the surface structures increasing the effective contact area, are the leading reasons for a superior triboelectric performance.
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| 7. |
- Dahlström, Christina, 1977-, et al.
(författare)
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Triboelectric Performance Of Regenerated Cellulose
- 2023
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Ingår i: Book of Abstracts EPNOE 2023. - : Graz University of Technology. ; , s. 116-
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Konferensbidrag (övrigt vetenskapligt/konstnärligt)abstract
- Cellulose has shown great potential in the development of green triboelectric nanogenerators (TENG) [1]. Particularly, regenerated cellulose (R-cellulose) has shown remarkably high output power density but the structural features and key parameters that explain such superior performance remain unexplored. In this work, wood cellulose fibers were dissolved in a LiOH(aq)-based solvent to produce a series of R-cellulose films. Regeneration in different alcohols (from methanol to n-pentanol) was performed and the films’ structural features and triboelectric performance were assessed. Nonsolvents of increased hydrophobicity led to R-cellulose films with higher hydrophilic character; the films showed a (1- 10) diffraction peak of larger amplitude and higher apparent crystallinity. An open-circuit voltage (VOC) of up to ca. 260 V and a short-circuit current (ISC) of up to ca. 150 μA were measured for R-cellulose against polytetrafluoroethylene (as negative counter-layer). However, R-cellulose showed an increased VOC of 175% (from 88.1 V) against polydimethylsiloxane from methanol to n-pentanol. The corresponding ISC and output power also increased by 76% (from 89.9 μA) and by 382% (from 8.8 W m–2), respectively. The higher R-cellulose hydrophilicity, combined with soft counter-layer that follow the surface structures increasing the effective contact area, are the leading reasons for a superior triboelectric performance.[1] Zhang, R., Dahlström, C., Zou, H., Jonzon, J., Hummelgård, M., Örtegren, J., Blomquist, N., Yang, Y., Andersson, H., Olsen, M., Norgren, M., Olin, H. & Wang, Z.L. Adv. Mater. 32, 2002824, 2020; https://doi.org/10.1002/adma.202002824
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| 8. |
- Duarte, H., et al.
(författare)
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On the Valorization of Arbutus unedo L. Pomace : Polyphenol Extraction and Development of Novel Functional Cookies
- 2023
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Ingår i: Foods. - : MDPI. - 2304-8158. ; 12:19
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Tidskriftsartikel (refereegranskat)abstract
- The fruits of Arbutus unedo L. have a crimson colour and are enriched with remarkable concentrations of bioactive compounds such as anthocyanins and polyphenols. These fruits are commonly used in the production of a Portuguese Protected Geographical Indication distillate called “Aguardente de Medronho”. During this process, a solid pomace is generated and presently discarded without valuable applications. In this work, two strategies have been developed for the valorisation of A. unedo pomace. The first approach considers the extraction of polyphenols from this by-product through the optimization of an ultrasound-assisted method using a Box-Behnken design coupled with response surface methodology. The results indicate that the temperature and the percentage of methanol, along with their interaction, significantly influence the total concentration of polyphenols and the antioxidant activity of the extracts obtained. The optimal conditions identified consider the extraction of 0.5 g of sample with 20 mL of a solvent containing 74% MeOH (aq), at a pH of 4.8, maintained at 70 °C for 15 min. On the other hand, the second valorisation strategy considered the use of A. unedo pomace in the development of functional cookies. The incorporation of 15–20% pomace in the cookie formulation was well-received by consumers. This incorporation results in an intake of ca. 6.55 mg of polyphenols per gram of cookie consumed, accompanied by an antioxidant activity of 4.54 mg Trolox equivalents per gram of cookie consumed. Overall, these results encourage the employment of A. unedo pomace either as a reliable source of extracts enriched in polyphenols or as a nutraceutical active ingredient in functional cookies, thereby positively impacting human health.
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| 9. |
- Duarte, H., et al.
(författare)
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Optimization of the extraction of polyphenols from Pinus pinaster residues using deep eutectic solvents : a sustainable approach
- 2023
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Ingår i: Wood Science and Technology. - : Springer Nature. - 0043-7719 .- 1432-5225. ; 57:5, s. 1175-1196
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Tidskriftsartikel (refereegranskat)abstract
- Abstract: In the present investigation, the optimization of a pressurized solid–liquid extraction of polyphenols from Pinus pinaster Aiton needles and bark residues has been carried out using new deep eutectic solvent systems (DES). A Box–Behnken design with response surface methodology was implemented, with six variables, including solid:liquid ratio, water content, temperature, extraction time, reactor closure state, and catalyst concentration. The DES consisting of levulinic acid: formic acid exhibited the highest content, and the optimal conditions were determined to be 0.10 g of residue in 10 mL of solvent (without water) and without catalyst, at 60 °C for 5 min. The method demonstrated excellent repeatability and intermediate precision, with a coefficient of variation of less than 5%. In addition, the antimicrobial and antioxidant activities of the polyphenol-enriched extracts were evaluated, obtaining a total reduction in S. aureus cell growth and remarkable antioxidant levels of 144.72 ± 4.24 and 161.01 ± 4.70 mg Trolox equivalents/gram for needle and bark residues, respectively. Under the optimized conditions, the new DES are remarkably superior to conventional solvents and can be recycled and reused, demonstrating that these systems have a promising environmental profile, making them valuable alternatives for biomass fractionation.
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| 10. |
- Duarte, H., et al.
(författare)
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Sustainable extraction of polyphenols from vine shoots using deep eutectic solvents : Influence of the solvent, Vitis sp., and extraction technique
- 2024
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Ingår i: Talanta. - : Elsevier BV. - 0039-9140 .- 1873-3573. ; 267
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Tidskriftsartikel (refereegranskat)abstract
- Vine shoots are the main by-products of grapevine pruning with no added value. In the present study, deep eutectic solvents (DESs) were used as alternatives to traditional chemical solvents, for the extraction of phytochemicals from grapevine shoots. Three levulinic acid-based DESs were tested for the first time, and their performance was compared to methanol (a standard chemical solvent) regarding the extraction of phenolic compounds from thirteen Vitis sp. shoots. Two extraction methods have been applied: ultrasound-assisted extraction and solid-liquid extraction. A total of eleven polyphenols which belongs to four families (proanthocyanins, stilbenes, hydroxycinnamic acids, and flavonols) have been identified and quantified in the extracts. The statistical analysis shows that the levulinic acid-based DES systems are novel and important alternatives to chemical solvents due to favourable eco-friendly properties and remarkable extraction performance of polyphenols. On the other hand, the ultrasound-assisted extraction technique has significantly increased the extraction rate in comparison to the solid-liquid extraction method with p-values lower than 0.05 for most compounds. The genetic factor has been shown to play an important role in the content of extracted polyphenols, being V. riparia pubescente the one that presented the highest concentrations of extracted polyphenols. Finally, the polyphenol-enriched extracts have proven important properties such as antioxidant activity and significant delay in bacteria growth against both gram-positive and gram-negative bacteria. It is important to note that, to the best of our knowledge, this is the first time that deep eutectic solvents have been used for the extraction of bioactive compounds from vine shoot residues.
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