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Advances in Inorganic Chemistry, Volume 57 - 1st Edition
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Free Relaxometry Of Water Metal Ion Interactions
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The smaller NPs' size without CA At higher polymer concentration 0. The morphology of the NPs observed revealed that the particles are spherical in shape and monodisperse Figure S5. The higher encapsulation results for 0. The zeta potential value of the 0. IR measurements were also performed Figure S6. T 1 and T 2 measurements at 60 MHz 1. Relaxivity results obtained at MHz are presented on a per millimolar Gd basis in Figure 8 and show a maximum r 1 of Even though all the proposed formulations of Gd-DTPA-loaded HA nanostructures show an increase of the r 1 signal, as reported in Figure 7 A, the highest boosting of the relaxivity is provided by the NPs obtained using the formulation at 0.
Loaded NPs perform far better even compared to the unloaded ones, whose distribution appears to be broad and centered around ms. It is worth mentioning that, compared to T 1 distribution for bulk water ms , unloaded NPs' distribution shows that a slight contribution to the longitudinal relaxivity is ascribable to the crosslinked polymer nanostructure, which is able by itself to tune the water mobility for a non-nanostructured material.
The contribution, therefore, to the overall relaxivity is further enhanced in the ternary system, thanks to the water-mediated interaction between the polymer and metal chelate. The NMRD profiles as a function of the static magnetic field of the aqueous solutions of Gd-DTPA and loaded and unloaded NPs Figure 8 are set up to establish the effects caused by Hydrodenticity functionalities on the parameters that determine the observed relaxivities.
Conversely, longitudinal relaxivity r 1 for loaded NPs HA at 0.
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As a control, unloaded NPs do not exhibit increase in relaxivity in this field region, confirming that the nanohydrogel structure containing Gd-DTPA contributes to slowing the chelator's tumbling motion and allows water exchange thanks to its hydrophilic properties, as hypothesized in the concept of Hydrodenticity.
This work reports the use of polymer hydrogels for boosting the relaxivity of clinical relevant CAs.
It is already known that, in an aqueous polymer solution, solvent affinity can alter polymer conformation by inducing local solvation of the structure that influences the number of available conformations of the polymer chains. Moreover, the introduction of another soluble ionic component, such as Gd-DTPA, in the system can induce further changes in polymer conformation, detectable via diverse thermodynamic approaches [ 74 - 77 ]. Based on our findings, we prove for the first time that these conformational changes, induced by the metal chelate, contribute to an increase in CA's relaxivity.
In fact, the high porosity of the hydrogel, which shows a mesh-like structure, is controlled by varying the density of covalent crosslinking [ 78 , 79 ]. Moreover, the presence of negatively charged groups and the degree of crosslinking influence water adsorption capacity and, thus, the relaxometric properties of the ternary system [ 45 ]. Therefore, the presence of the hydrogel matrix can significantly amplify the magnetic properties of the encapsulated Gd-DTPA, suggesting a strong outer-sphere and second-sphere contribution to the relaxivity. Based on these observations, we hypothesize that increased relaxivity is mainly related to the creation of water domains or clusters water compartments around the CA within the polymer matrix.
In fact, biopolymer systems contain intermolecular cavities that can be considered as molecular nano-domains in which various self-assembly processes can be implemented in principle [ 80 ]. The formation of peculiar structures within these cavities can be associated with thermodynamic transitions and it is a characteristic of many metallopolymer systems [ 81 , 82 ]. The entrapment of the CA inside the hydrophilic matrix of HA results in a reduction of the rotational tumbling rate, due to an increase of the effective viscosity of the aqueous solution into the hydrogel matrix.
At the same time, multiple CA-water interaction pathways occur between the exchangeable protons of the water molecules coordinated by the CA and the other water molecules freely moving within the hydrogel mesh or bonded to the polymer chains [ 22 , 44 , 83 ]. The so created nanostructure is composed of different water layers departing from the polymer chains that surround the Gd-molecules. It is known, in fact, that hydrated polysaccharides, such as HA, are characterized by the presence of multiple water layers, contiguous regions of variable water density within a polyelectrolyte solution [ 84 ], differing in their physical properties depending on the distance from the polysaccharide chain [ 85 ].
In addition, the developed polymer network can be dependent not only on the water layers organization but also on other solute species, such as Gd-DTPA, altering the bound water layer with non-negligible effect on the HA conformation and dynamic [ 86 ].