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Keywords = MQ-NMR

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24 pages, 2980 KiB  
Article
Effect of Proteins on the Network Formation and Degradation of Peroxide Cross-Linked Natural Rubber Elucidated by Time-Domain NMR
by Adun Nimpaiboon, Antonio González-Jiménez, Roberto Pérez-Aparicio, Fernando Martín-Salamanca, Zenen Zepeda-Rodríguez, Juan López-Valentín and Jitladda Sakdapipanich
Polymers 2025, 17(8), 1063; https://doi.org/10.3390/polym17081063 - 15 Apr 2025
Viewed by 652
Abstract
The importance of sustainable polymers has increased greatly in the last years since most polymers are derived from non-renewable sources. Sustainable polymers (i.e., biopolymers) such as natural rubber (NR) are proposed as a solution for this concern. A comparative study between NR and [...] Read more.
The importance of sustainable polymers has increased greatly in the last years since most polymers are derived from non-renewable sources. Sustainable polymers (i.e., biopolymers) such as natural rubber (NR) are proposed as a solution for this concern. A comparative study between NR and deproteinized NR (DPNR) was carried out to elucidate the role of proteins on the network formation and degradation of peroxide cross-linked NR using time-domain NMR experiments. The 1H multiple-quantum (MQ) NMR experiments provided information on the cross-link density and its spatial distribution, while the actual fraction of non-coupled network defects was obtained by exploiting the Hahn echo approach measured on swollen samples. The results showed that proteins influenced the network formation during the vulcanization process of NR, leading to a higher number of non-elastic network defects and promoting the creation of additional cross-links with a broader spatial distribution. The formation of network heterogeneities in different length scales deeply influences the mechanical properties of NR samples. On the other hand, the proteins showed a pro-oxidant activity on the degradation behavior by accelerating the degradation process of peroxide cross-linked NR. Full article
(This article belongs to the Special Issue Exploration and Innovation in Sustainable Rubber Performance)
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16 pages, 6355 KiB  
Article
Solid-State NMR Characterization of Mefloquine Resinate Complexes Designed for Taste-Masking Pediatric Formulations
by Leandro B. Borré, Eduardo G. R. Sousa, Rosane A. S. San Gil, Mateus M. Baptista, Alexandre A. Leitão, João M. A. R. De Almeida, Olívia Carr, Osvaldo N. Oliveira, Flávio M. Shimizu and Thiago F. Guimarães
Pharmaceuticals 2024, 17(7), 870; https://doi.org/10.3390/ph17070870 - 2 Jul 2024
Viewed by 1243
Abstract
Mefloquine (MQ) is an antimalarial medication prescribed to treat or malaria prevention.. When taken by children, vomiting usually occurs, and new doses of medication frequently need to be taken. So, developing pediatric medicines using taste-masked antimalarial drug complexes is mandatory for the success [...] Read more.
Mefloquine (MQ) is an antimalarial medication prescribed to treat or malaria prevention.. When taken by children, vomiting usually occurs, and new doses of medication frequently need to be taken. So, developing pediatric medicines using taste-masked antimalarial drug complexes is mandatory for the success of mefloquine administration. The hypothesis that binding mefloquine to an ion-exchange resin (R) could circumvent the drug’s bitter taste problem was proposed, and solid-state 13C cross-polarization magic angle spinning (CPMAS) NMR was able to follow MQ–R mixtures through chemical shift and relaxation measurements. The nature of MQ–R complex formation could then be determined. Impedimetric electronic tongue equipment also verified the resinate taste-masking efficiency in vitro. Variations in chemical shifts and structure dynamics measured by proton relaxation properties (e.g., T1ρH) were used as probes to follow the extension of mixing and specific interactions that would be present in MQ–R. A significant decrease in T1ρH values was observed for MQ carbons in MQ–R complexes, compared to the ones in MQ (from 100–200 ms in MQ to 20–50 ms in an MQ–R complex). The results evidenced that the cationic resin interacts strongly with mefloquine molecules in the formulation of a 1:1 ratio complex. Thus, 13C CPMAS NMR allowed the confirmation of the presence of a binding between mefloquine and polacrilin in the MQ–R formulation studied. Full article
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14 pages, 787 KiB  
Article
Introducing “MEW2” Software: A Tool to Analyze MQ-NMR Experiments for Elastomers
by Fernando M. Salamanca, Zenen Zepeda-Rodríguez, Laura Diñeiro, Marina M. Escrivá, Rebeca Herrero, Rodrigo Navarro and Juan L. Valentín
Polymers 2023, 15(20), 4058; https://doi.org/10.3390/polym15204058 - 11 Oct 2023
Cited by 1 | Viewed by 1886
Abstract
Low-field time-domain proton Nuclear Magnetic Resonance (NMR) spectroscopy is an attractive and powerful tool for studying the structure and dynamics of elastomers. The existence of crosslinks and other topological constraints in rubber matrices (entanglements and filler–rubber interactions, among others) renders the fast segmental [...] Read more.
Low-field time-domain proton Nuclear Magnetic Resonance (NMR) spectroscopy is an attractive and powerful tool for studying the structure and dynamics of elastomers. The existence of crosslinks and other topological constraints in rubber matrices (entanglements and filler–rubber interactions, among others) renders the fast segmental fluctuations of the polymeric chains non-isotropic, obtaining nonzero residual dipolar couplings, which is the main observable of MQ-NMR experiments. A new software, Multiple quantum nuclear magnetic resonance analyzer for Elastomeric Networks v2 (MEW2), provides a new tool to facilitate the study of the molecular structure of elastomeric materials. This program quantitatively analyzes two different sets of experimental data obtained in the same experiment, which are dominated by multiple-quantum coherence and polymer dynamics. The proper quantification of non-coupled network defects (dangling chain ends, loops, etc.) allows the analyzer to normalize the multiple quantum intensity, obtaining a build-up curve that contains the structural information without any influence from the rubber dynamics. Finally, it provides the spatial distribution of crosslinks using a fast Tikhonov regularization process based on a statistical criterion. As a general trend, this study provides an automatic solution to a tedious procedure of analysis, demonstrating a new tool that accelerates the calculations of network structure using 1H MQ-NMR low-field time-domain experiments for elastomeric compounds. Full article
(This article belongs to the Special Issue Advances in Rubbers)
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