Solution NMR methods for structural and thermodynamic investigation of nanoparticle adsorption equilibria

An, Yeongseo; Sedinkin, Sergey L.; Venditti, Vincenzo

doi:10.1039/d2na00099g

Cited by 12 publications

(21 citation statements)

References 230 publications

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“…When a solution-state molecule interacts weakly with a large receptor, the relaxation rate observed in solution will be a weighted average of the relaxation rate of the free and bound molecules. Since the relaxation of the bound state is expected to be significantly faster than that of the free state, the longer the molecule spends in the bound state, the shorter the observed T 2 relaxation time will be. , …”

Section: Results and Discussionmentioning

confidence: 99%

“…Since the relaxation of the bound state is expected to be significantly faster than that of the free state, the longer the molecule spends in the bound state, the shorter the observed T 2 relaxation time will be. 56,62 The line broadening observed in Figure 2a−c prompted us to undertake a systematic study of the T 2 relaxation times of each sample. The measured R 2 relaxation rates (R 2 = 1/T 2 ) as a function of added nanoparticle concentration for each antibiotic are shown in Figure 3.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Many field − and laboratory − studies have been undertaken in order to quantify the amount and types of small molecule xenobiotics interacting with plastic in the environment, yet few studies are aimed at understanding the mechanism of sorption. However, NMR spectroscopy is a powerful technique for atomic-level structure determination, and has been extensively used to study small molecules interacting with nanoparticles in both the solid state − and solution state. − Different NMR experiments can provide complementary information about nanoparticle-small molecule binding, leading to an overall picture of the binding mechanism. This understanding is important in developing structure–activity relationships for binding between small molecules and large plastic particles.…”

Section: Introductionmentioning

confidence: 99%

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Binding Between Antibiotics and Polystyrene Nanoparticles Examined by NMR

et al. 2022

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Elucidating the interactions between plastic nanoparticles and small molecules is important to understanding these interactions as they occur in polluted waterways. For example, plastic that breaks down into micro-and nanoscale particles will interact with small molecule pollutants that are also present in contaminated waters. Other components of natural water, such as dissolved organic matter, will also influence these interactions. Here we use a collection of complementary NMR techniques to examine the binding between polystyrene nanoparticles and three common antibiotics, belonging to a class of molecules that are expected to be common in polluted water. Through examination of proton NMR signal intensity, relaxation times, saturation-transfer difference (STD) NMR, and competition STD-NMR, we find that the antibiotics have binding strengths in the order amoxicillin < metronidazole ≪ levofloxacin. Levofloxacin is able to compete for binding sites, preventing the other two antibiotics from binding. The presence of tannic acid disrupts the binding between levofloxacin and the polystyrene nanoparticles, but does not influence the binding between metronidazole and these nanoparticles.

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Section: Results and Discussionmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Binding Between Antibiotics and Polystyrene Nanoparticles Examined by NMR

et al. 2022

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“…2b), and considerable spectral narrowing. The temperature-dependent spectral narrowing and chemical shift can be explained by the dynamic equilibrium between 1 and 2 49,50 . This equilibrium is biased to 1 at room temperature and shifts toward 2 as the temperature decreases.…”

Section: Surface Reaction Of Precursors and Intermediate Speciesmentioning

confidence: 99%

Heteroepitaxial chemistry of zinc chalcogenides on InP nanocrystals for defect-free interfaces with atomic uniformity

et al. 2023

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Heteroepitaxy on colloidal semiconductor nanocrystals is an essential strategy for manipulating their optoelectronic functionalities. However, their practical synthesis typically leads to scattered and unexpected outcomes due to the intervention of multiple reaction pathways associated with complicated side products of reactants. Here, the heteroepitaxy mechanism of zinc chalcogenide initiated on indium phosphide (InP) colloidal nanocrystals is elucidated using the precursors, zinc carboxylate and trialkylphosphine selenide. The high magnetic receptivity of 77Se and the characteristic longitudinal optical phonon mode of ZnSe allowed for monitoring the sequence of epilayer formation at the molecular level. The investigation revealed the sterically hindered acyloxytrialkylphosphonium and diacyloxytrialkylphosphorane to be main intermediates in the surface reaction, which retards the metal ion adsorption by a large steric hindrance. The transformation of adsorbates to the crystalline epilayer was disturbed by surface oxides. Raman scattering disclosed the pathway of secondary surface oxidation triggered by carboxylate ligands migrated from zinc carboxylate. The surface-initiated heteroepitaxy protocol is proposed to fabricate core/shell heterostructured nanocrystals with atomic-scale uniformity of epilayers. Despite the large lattice mismatch of ZnS to InP, we realised a uniform and interface defect-free ZnS epilayer (~0.3 nm thickness) on InP nanocrystals, as evidenced by a high photoluminescence quantum yield of 97.3%.

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“…Solid-state NMR has been used extensively to characterize nanoparticle–ligand interactions. − Recently, several novel solution-state NMR methods have been used to gain information on these kinds of interactions as well. ,− Comprehensive multiphase (CMP) NMR, on the other hand, is the only method that can simultaneously probe solid, liquid, and gel-like phases in an intact sample . A CMP-NMR probe contains the ability to handle the high RF power required for solid-state NMR, as well as a lock, pulse field gradient, and susceptibility matching required for both solution and gel-state NMR.…”

Section: Introductionmentioning

confidence: 99%

Comprehensive Multiphase NMR Examination of Amino Acids Binding to the Dynamic Shell of Polystyrene Nanoparticles to Understand Environmental Hazards Associated with Nanoscale Plastic

Biswas

Soong

Schmidig

et al. 2022

ACS Appl. Nano Mater.

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Plastic pollution is a growing environmental concern. In addition to posing hazards to wildlife, micro- and nano-scale plastic particles can adsorb toxic small molecules from polluted waterways, which may be released when these plastic particles are ingested by animals or humans. Previous NMR studies have examined the binding between surface-modified polystyrene nanoparticles and amino acids as models for small molecules with a variety of functional groups. These previous studies, however, could only examine the liquid phase and therefore focused on the small molecules. In the current study, we use comprehensive multiphase NMR (CMP-NMR) to examine both the small molecules and polystyrene nanoparticles in all phases including liquid, solid, and gel-like phases. Through proton spectral editing techniques and 13C solid-state NMR experiments, we find that the polystyrene nanoparticles contain both solid and gel-like fractions. The bound amino acid exists primarily in the gel-like phase, with very little amino acid existing in the true solid phase. This suggests that the bound amino acid interacts with the nanoparticle shell rather than the solid-like core. These experiments relied on the ability of CMP-NMR to separately observe the solid, liquid, and gel-like phases of the same sample and demonstrate the complementary nature of this approach for understanding complex multiphase systems.

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Solution NMR methods for structural and thermodynamic investigation of nanoparticle adsorption equilibria

Abstract: Characterization of dynamic processes occurring at the nanoparticle (NP) surface is crucial for developing new and more efficient NP catalysts and materials. Thus, a vast amount of research has been...

Cited by 12 publications

References 230 publications

Binding Between Antibiotics and Polystyrene Nanoparticles Examined by NMR

Binding Between Antibiotics and Polystyrene Nanoparticles Examined by NMR

Heteroepitaxial chemistry of zinc chalcogenides on InP nanocrystals for defect-free interfaces with atomic uniformity

Comprehensive Multiphase NMR Examination of Amino Acids Binding to the Dynamic Shell of Polystyrene Nanoparticles to Understand Environmental Hazards Associated with Nanoscale Plastic

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