Biodegradable Nanoparticles Loaded with Levodopa and Curcumin for Treatment of Parkinson’s Disease

Background: Parkinson’s disease (PD) is the second most common age-related neurodegenerative disorder. Levodopa (L-DOPA) remains the gold-standard drug available for treating PD. Curcumin has many pharmacological activities, including antioxidant, anti-inflammatory, antimicrobial, anti-amyloid, and antitumor properties. Copolymers composed of Poly (ethylene oxide) (PEO) and biodegradable polyesters such as Poly (ε-caprolactone) (PCL) can self-assemble into nanoparticles (NPs). This study describes the development of NH₂–PEO–PCL diblock copolymer positively charged and modified by adding glutathione (GSH) on the outer surface, resulting in a synergistic delivery of L-DOPA curcumin that would be able to pass the blood–brain barrier. Methods: The NH₂–PEO–PCL NPs suspensions were prepared by using a nanoprecipitation and solvent displacement method and coated with GSH. NPs were submitted to characterization assays. In order to ensure the bioavailability, Vero and PC12 cells were treated with various concentrations of the loaded and unloaded NPs to observe cytotoxicity. Results: NPs have successfully loaded L-DOPA and curcumin and were stable after freeze-drying, indicating advancing into in vitro toxicity testing. Vero and PC12 cells that were treated up to 72 h with various concentrations of L-DOPA and curcumin-loaded NP maintained high viability percentage, indicating that the NPs are biocompatible. Conclusions: NPs consisting of NH₂–PEO–PCL were characterized as potential formulations for brain delivery of L-DOPA and curcumin. The results also indicate that the developed biodegradable nanomicelles that were blood compatible presented low cytotoxicity.     

The Peptide Functionalized Inorganic Nanoparticles for Cancer-Related Bioanalytical and Biomedical Applications

In order to improve their bioapplications, inorganic nanoparticles (NPs) are usually functionalized with specific biomolecules. Peptides with short amino acid sequences have attracted great attention in the NP functionalization since they are easy to be synthesized on a large scale by the automatic synthesizer and can integrate various functionalities including specific biorecognition and therapeutic function into one sequence. Conjugation of peptides with NPs can generate novel theranostic/drug delivery nanosystems with active tumor targeting ability and efficient nanosensing platforms for sensitive detection of various analytes, such as heavy metallic ions and biomarkers. Massive studies demonstrate that applications of the peptide–NP bioconjugates can help to achieve the precise diagnosis and therapy of diseases. In particular, the peptide–NP bioconjugates show tremendous potential for development of effective anti-tumor nanomedicines. This review provides an overview of the effects of properties of peptide functionalized NPs on precise diagnostics and therapy of cancers through summarizing the recent publications on the applications of peptide–NP bioconjugates for biomarkers (antigens and enzymes) and carcinogens (e.g., heavy metallic ions) detection, drug delivery, and imaging-guided therapy. The current challenges and future prospects of the subject are also discussed.     

Structure observation of graphene quantum dots by single-layered formation in layered confinement space

Graphene quantum dots (GQDs) have received much research attention due to their unique optical/electrical/magnetic features. However, the intrinsic relationship between the structure and properties of GQDs remains not fully understood, because the controlled synthesis and the accurate structure determination of GQDs are still a great challenge. Here, single-layered GQDs are successfully obtained by the hydrothermal treatment of intercalated citrate in the confined space of 2D interlayer galleries of layered double hydroxides (LDHs). The distinct molecular structures of the single-layered GQDs reveal that the blue photoluminescence of the GQDs derives from a rigid π-conjugate plane structure, which is in accordance with theoretical calculations. This work will open the door towards a quantitative understanding of the structure-property effects of GQDs.     

Tuning the singlet-triplet energy gap: a unique approach to efficient photosensitizers with aggregation-induced emission (AIE) characteristics

The efficiency of the intersystem crossing process can be improved by reducing the energy gap between the singlet and triplet excited states (ΔE _ST), which offers the opportunity to improve the yield of the triplet excited state. Herein, we demonstrate that modulation of the excited states is also an effective strategy to regulate the singlet oxygen generation of photosensitizers. Based on our previous studies that photosensitizers with aggregation-induced emission characteristics (AIE) showed enhanced fluorescence and efficient singlet oxygen production in the aggregated state, a series of AIE fluorogens such as TPDC, TPPDC and PPDC were synthesized, which showed ΔE _ST values of 0.48, 0.35 and 0.27 eV, respectively. A detailed study revealed that PPDC exhibited the highest singlet oxygen efficiency (0.89) as nanoaggregates, while TPDC exhibited the lowest efficiency (0.28), inversely correlated with their ΔE _ST values. Due to their similar optical properties, TPDC and PPDC were further encapsulated into nanoparticles (NPs). Subsequent surface modification with cell penetrating peptide (TAT) yielded TAT–TPDC NPs and TAT–PPDC NPs. As a result of the stronger singlet oxygen generation, TAT–PPDC NPs showed enhanced cancer cell ablation as compared to TAT–TPDC NPs. Fine-tuning of the singlet-triplet energy gap is thus proven to be an effective new strategy to generate efficient photosensitizers for photodynamic therapy.     

Solar-microbial hybrid device based on oxygen-deficient niobium pentoxide anodes for sustainable hydrogen production

Hydrogen gas is emerging as an attractive fuel with high energy density for the direction of energy resources in the future. Designing integrated devices based on a photoelectrochemical (PEC) cell and a microbial fuel cell (MFC) represents a promising strategy to produce hydrogen fuel at a low price. In this work, we demonstrate a new solar-microbial (PEC–MFC) hybrid device based on the oxygen-deficient Nb₂O₅ nanoporous (Nb₂O_5–x NPs) anodes for sustainable hydrogen generation without external bias for the first time. Owing to the improved conductivity and porous structure, the as-prepared Nb₂O_5–x NPs film yields a remarkable photocurrent density of 0.9 mA cm^–2 at 0.6 V (vs. SCE) in 1 M KOH aqueous solution under light irradiation, and can achieve a maximum power density of 1196 mW m^–2 when used as an anode in a MFC device. More importantly, a solar-microbial hybrid system by combining a PEC cell with a MFC is designed, in which the Nb₂O_5–x NPs electrodes function as both anodes. The as-fabricated PEC–MFC hybrid device can simultaneously realize electricity and hydrogen using organic matter and solar light at zero external bias. This novel design and attempt might provide guidance for other materials to convert and store energy.     

Using Aggregation to Chaperone Nanoparticles Across Fluid Interfaces

Nanoparticles (NPs) transfer is usually induced by adding ligands to modify NP surfaces, but aggregation of NPs oftentimes hampers the transfer. Here, we show that aggregation during NP phase transfer does not necessarily result in transfer failure. Using a model system comprising gold NPs and amphiphilic polymers, we demonstrate an unusual mechanism by which NPs can undergo phase transfer from the aqueous phase to the organic phase via a single-aggregation-single pathway. Our discovery challenges the conventional idea that aggregation inhibits NP transfer and provides an unexpected pathway for transferring larger-sized NPs (>20 nm). The charged amphiphilic polymers effectively act as chaperons for the NP transfer and offer a unique way to manipulate the dispersion and distribution of NPs in two immiscible liquids. Moreover, by intentionally jamming the NP-polymer assembly at the liquid/liquid interface, the transfer process can be inhibited.     

MWCNTs/Ionic Liquid/Graphene Quantum Dots Nanocomposite Coated with Nickel‐Cobalt Bimetallic Catalyst as a Highly Selective Non‐enzymatic Sensor for Determination of Glucose

In this work, a glassy carbon electrode (GCE) was modified with multiwall carbon nanotubes/ionic liquid/graphene quantum dots (MWCNTs/IL/GQDs) nanocomposite. Then, the nanocomposite was decorated with nickel‐cobalt nanoparticles (Ni?Co NPs), and it was used as a non‐enzymatic glucose sensor. Field emission scanning electron microscopy, X‐ray diffraction spectroscopy, and energy dispersive spectroscopy were employed to prove the electrodeposition of the Ni?Co NPs on the surface of MWCNTs/IL/GQDs/GCE. Also, cyclic voltammetric and amperometric methods were utilized for the investigation of the electrochemical behaviour of the Ni?Co NPs/MWCNTs/IL/GQDs/GCE for glucose oxidation. The novel amperometric sensor displayed two linear ranges from 1.0 to 190.0 μmol L^?1 and 190.0 to 4910 μmol L^?1 with a low detection limit of 0.3 μmol L^?1 as well as fast response time (2 s) and high stability. Also, the sensor showed good selectivity for glucose determination in the presence of ascorbic acid, citric acid, dopamine, uric acid, fructose, and sucrose, as potential interference species. Finally, the performance of the proposed sensor was investigated for the glucose determination in real samples. Ni?Co NPs/MWCNTs/IL/GQDs/GCE showed good sensitivity and excellent selectivity.     

Taming C60 fullerene: tuning intramolecular photoinduced electron transfer process with subphthalocyanines

Two subphthalocyanine–C₆₀ conjugates have been prepared by means of the 1,3-dipolar cycloaddition reaction of (perfluoro) or hexa(pentylsulfonyl) electron deficient subphthalocyanines to C₆₀. Comprehensive assays regarding the electronic features – in the ground and excited state – of the resulting conjugates revealed energy and electron transfer processes upon photoexcitation. Most important is the unambiguous evidence – in terms of time-resolved spectroscopy – of an ultrafast oxidative electron transfer evolving from C₆₀ to the photoexcited subphthalocyanines. This is, to the best of our knowledge, the first case of an intramolecular oxidation of C₆₀ within electron donor–acceptor conjugates by means of only photoexcitation.     

Catalysis of water oxidation in acetonitrile by iridium oxide nanoparticles

Water oxidation catalysed by iridium oxide nanoparticles (IrO₂ NPs) in water–acetonitrile mixtures using [Ru^III(bpy)₃]³⁺ as oxidant was studied as a function of the water content, the acidity of the reaction media and the catalyst concentration. It was observed that under acidic conditions (HClO₄) and at high water contents (80% (v/v)) the reaction is slow, but its rate increases as the water content decreases, reaching a maximum at approximately equimolar proportions (≈25% H₂O (v/v)). The results can be rationalized based on the structure of water in water–acetonitrile mixtures. At high water fractions, water is present in highly hydrogen-bonded arrangements and is less reactive. As the water content decreases, water clustering gives rise to the formation of water-rich micro-domains, and the number of bonded water molecules decreases monotonically. The results presented herein indicate that non-bonded water present in the water micro-domains is considerably more reactive towards oxygen production. Finally, long term electrolysis of water–acetonitrile mixtures containing [Ru^II(bpy)₃]²⁺ and IrO₂ NPs in solution show that the amount of oxygen produced is constant with time demonstrating that the redox mediator is stable under these experimental conditions.     

Charge trapping and storage by composite P3HT/PC60BM nanoparticles investigated by fluorescence-voltage/single particle spectroscopy

Fluorescence-voltage/single particle spectroscopy (F-V/SPS) was employed to study exciton-hole polaron interactions and interfacial charge transfer processes for pure poly(3-hexylthiophene) (P3HT) nanoparticles (NPs) and composite P3HT/PC(60)BM NPs in functioning hole-injection devices. F-V/SPS data collected on a particle-by-particle basis reveal an apparent bistability in the fluorescence-voltage modulation curves for composite NPs of P3HT and [6,6]-phenyl-C(61)-butyric acid methyl ester (PC(60)BM) that is absent for pure P3HT NPs. A pronounced deep trapping of free electrons photogenerated from the composite P3HT/PC(60)BM NPs at the NP/dielectric interface and hole trapping by fullerene anions in composite P3HT/PC(60)BM NPs under photoexcitation lies at the basis of this finding. The deep electron trapping effect reported here for composite conjugated polymer/fullerene NPs presents an opportunity for future application of these NPs in nanoscale memory and imaging devices.     

Synthesis of open-mouthed,yolk–shell Au@AgPd nanoparticles with access to interior surfaces for enhanced electrocatalysis

We have successfully produced open-mouthed, yolk–shell (OM-YS) Au@AgPd nanoparticles (NPs) via galvanic replacement reaction at room temperature; each NP has a large opening on its AgPd shells. Owing to the openings on the AgPd shells, the inner surfaces of the AgPd shells of as-prepared OM-YS Au@AgPd NPs become accessible to the surrounding media. These new structural characters make the present OM-YS Au@AgPd NPs excellent catalysts for electrochemical oxidation of ethanol in alkaline media. Their electrochemical active surface area is 87.8 m² g^–1 and the mass activity is 1.25 A mg_Pd^–1. Moreover, the openings on the AgPd shells also make the surfaces of the Au cores in OM-YS Au@AgPd NPs accessible to the reaction media, which significantly facilitates the removal of CO and other carbonaceous intermediate species, thus leading to substantially enhanced durability and stability. This superior electrocatalytic performance cannot be implemented by using conventional YS Au@AgPd NPs or commercially available Pd/C catalysts.     

Biogenic Synthesis of CuO,ZnO, and CuO–ZnO Nanoparticles Using Leaf Extracts of Dovyalis caffra and Their Biological Properties

Biogenic metal oxide nanoparticles (NPs) have emerged as a useful tool in biology due to their biocompatibility properties with most biological systems. In this study, we report the synthesis of copper oxide (CuO), zinc oxide (ZnO) nanoparticles (NPs), and their nanocomposite (CuO–ZnO) prepared using the phytochemical extracts from the leaves of Dovyalis caffra (kei apple). The physicochemical properties of these nanomaterials were established using some characterization techniques including X-ray diffraction analysis (XRD), ultraviolet-visible spectroscopy (UV-vis), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDX). The XRD result confirmed the presence of a monoclinic CuO (Tenorite), and a hexagonal ZnO (Zincite) nanoparticles phase, which were both confirmed in the CuO–ZnO composite. The electron microscopy of the CuO–ZnO, CuO, and ZnO NPs showed a mixture of nano-scale sizes and spherical/short-rod morphologies, with some agglomeration. In the constituent’s analysis (EDX), no unwanted peak was found, which showed the absence of impurities. Antioxidant properties of the nanoparticles was studied, which confirmed that CuO–ZnO nanocomposite exhibited better scavenging potential than the individual metal oxide nanoparticles (CuO, and ZnO), and ascorbic acid with respect to their minimum inhibitory concentration (IC₅₀) values. Similarly, the in vitro anticancer studies using MCF7 breast cancer cell lines indicated a concentration-dependent profile with the CuO–ZnO nanocomposite having the best activity over the respective metal oxides, but slightly lower than the standard 5-Fluorouracil drug.     

Multifunctional nanoparticles composite for MALDI-MS: Cd2+-doped carbon nanotubes with CdS nanoparticles as the matrix, preconcentrating and accelerating probes of microwave enzymatic digestion of peptides and proteins for direct MALDI-MS analysis

For the first time, we utilized multifunctional nanoparticles composite (NPs composite) for matrix-assisted laser desorption/ionization mass spectrometric (MALDI-MS) analysis of peptides and proteins. Multiwalled carbon nanotubes doped with Cd(2+) ions and modified with cadmium sulfide NPs were synthesized by a chemical reduction method at room temperature. The multifunctional NPs composite applied for the analysis of peptides and microwave-digested proteins in the atmospheric pressure matrix-assisted laser desorption/ionization ion-trap and MALDI time-of-flight (TOF) mass spectrometry (MS) was successfully demonstrated. The maximum detection sensitivity for peptides in MALDI-MS was achieved by the adsorption of negatively charged peptides onto the surfaces of NP composite through electrostatic interactions. The optimal conditions of peptide mixtures were obtained at 20 min of incubation time using 1 mg of NPs composite when the pH of the sample solution was kept higher than the pI values of peptides. The potentiality of the NP composite in the preconcentration of peptides was compared with that of the individual NP by calculating the preconcentration factors (PF) and found that the NPs composite showed a 4-6 times of PF than the other NPs. In addition, the NPs composite was also applied as heat-absorbing materials for efficient microwave tryptic digestion of cytochrome c and lysozyme from milk protein in MALDI-TOF-MS analysis. We believe that the use of NPs composite technique would be an efficient and powerful preconcentrating tool for MALDI-MS for the study of proteome research.     

Rational design of a “dual lock-and-key” supramolecular photosensitizer based on aromatic nucleophilic substitution for specific and enhanced photodynamic therapy

Photosensitizing agents are essential for precise and efficient photodynamic therapy (PDT). However, most of the conventional photosensitizers still suffer from limitations such as aggregation-caused quenching (ACQ) in physiological environments and toxic side-effects on normal tissues during treatment, leading to reduced therapeutic efficacy. Thus, integrating excellent photophysical properties and accurate carcinoma selectivity in a photosensitizer system remains highly desired. Herein, a “dual lock-and-key” supramolecular photosensitizer BIBCl–PAE NPs for specific and enhanced cancer therapy is reported. BIBCl–PAE NPs are constructed by encapsulating a rationally designed glutathione (GSH)-activatable photosensitizer BIBCl in a pH-responsive diblock copolymer. In normal tissues, BIBCl is “locked” in the hydrophobic core of the polymeric micelles due to ACQ. Under the “dual key” activation of low pH and high levels of GSH in a tumor microenvironment, the disassembly of micelles facilitates the reaction of BIBCl with GSH to release water-soluble BIBSG with ideal biocompatibility, enabling the highly efficient PDT. Moreover, benefiting from the Förster resonance energy transfer effect of BIBSG, improved light harvesting ability and ¹O₂ production are achieved. In vitro and vivo experiments have demonstrated that BIBCl–PAE NPs are effective in targeting and inhibiting carcinoma. BIBCl–PAE NPs show superior anticancer efficiency relative to non-activatable controls.

The “dual lock-and-key” supramolecular photosensitizers enable specific and enhanced photodynamic therapy (PDT).     

On the Hopping Efficiency of Nanoparticles in the Electron Transfer across Self‐Assembled Monolayers

Redox reactions of solvated molecular species at gold‐electrode surfaces modified by electrochemically inactive self‐assembled molecular monolayers (SAMs) are found to be activated by introducing Au nanoparticles (NPs) covalently bound to the SAM to form a reactive Au–alkanedithiol–NP–molecule hybrid entity. The NP appears to relay long‐range electron transfer (ET) so that the rate of the redox reaction may be as efficient as directly on a bare Au electrode, even though the ET distance is increased by several nanometers. In this study, we have employed a fast redox reaction of surface‐confined 6‐(ferrocenyl) hexanethiol molecules and NPs of Au, Pt and Pd to address the dependence of the rate of ET through the hybrid on the particular NP metal. Cyclic voltammograms show an increasing difference in the peak‐to‐peak separation for NPs in the order Au<Pt<Pd, especially when the length of the alkanedithiol increases from octanedithiol to decanedithiol. The corresponding apparent rate constants, k_app, for decanedithiol are 1170, 360 and 14 s^?1 for NPs of Au, Pt and Pd, respectively, indicating that the efficiency of NP mediation of the ET clearly depends on the nature of the NP. Based on a preliminary analysis rooted in interfacial electrochemical ET theory, combined with a simplified two‐step view of the NP coupling to the electrode and the molecule, this observation is referred to the density of electronic states of the NPs, reflected in a broadening of the molecular electron/NP bridge group levels and energy‐gap differences between the Fermi levels of the different metals.     

Preparation,Marriage Chemistry and Applications of Graphene Quantum Dots–Nanocellulose Composite: A Brief Review

Graphene quantum dots (GQDs) are zero-dimensional carbon-based materials, while nanocellulose is a nanomaterial that can be derived from naturally occurring cellulose polymers or renewable biomass resources. The unique geometrical, biocompatible and biodegradable properties of both these remarkable nanomaterials have caught the attention of the scientific community in terms of fundamental research aimed at advancing technology. This study reviews the preparation, marriage chemistry and applications of GQDs–nanocellulose composites. The preparation of these composites can be achieved via rapid and simple solution mixing containing known concentration of nanomaterial with a pre-defined composition ratio in a neutral pH medium. They can also be incorporated into other matrices or drop-casted onto substrates, depending on the intended application. Additionally, combining GQDs and nanocellulose has proven to impart new hybrid nanomaterials with excellent performance as well as surface functionality and, therefore, a plethora of applications. Potential applications for GQDs–nanocellulose composites include sensing or, for analytical purposes, injectable 3D printing materials, supercapacitors and light-emitting diodes. This review unlocks windows of research opportunities for GQDs–nanocellulose composites and pave the way for the synthesis and application of more innovative hybrid nanomaterials.     

Two dimensional inorganic electride-promoted electron transfer efficiency in transfer hydrogenation of alkynes and alkenes

A simple and highly efficient transfer hydrogenation of alkynes and alkenes by using a two-dimensional electride, dicalcium nitride ([Ca₂N]⁺·e^–), as an electron transfer agent is disclosed. Excellent yields in the transformation are attributed to the remarkable electron transfer efficiency in the electride-mediated reactions. It is clarified that an effective discharge of electrons from the [Ca₂N]⁺·e^– electride in alcoholic solvents is achieved by the decomposition of the electride via alcoholysis and the generation of ammonia and Ca(OⁱPr)₂. We found that the choice of solvent was crucial for enhancing the electron transfer efficiency, and a maximum efficiency of 80% was achieved by using a DMF mixed isopropanol co-solvent system. This is the highest value reported to date among single electron transfer agents in the reduction of C–C multiple bonds. The observed reactivity and efficiency establish that electrides with a high density of anionic electrons can readily participate in the reduction of organic functional groups.     

Post-synthetic halide conversion and selective halogen capture in hybrid perovskites

Reaction with halogen vapor allows us to post-synthetically exchange halides in both three- (3D) and two-dimensional (2D) organic–inorganic metal-halide perovskites. Films of 3D Pb–I perovskites cleanly convert to films of Pb–Br or Pb–Cl perovskites upon exposure to Br₂ or Cl₂ gas, respectively. This gas–solid reaction provides a simple method to produce the high-quality Pb–Br or Pb–Cl perovskite films required for optoelectronic applications. Reactivity with halogens can be extended to the organic layers in 2D metal-halide perovskites. Here, terminal alkene groups placed between the inorganic layers can capture Br₂ gas through chemisorption to form dibromoalkanes. This reaction''s selectivity for Br₂ over I₂ allows us to scrub Br₂ to obtain high-purity I₂ gas streams. We also observe unusual halogen transfer between the inorganic and organic layers within a single perovskite structure. Remarkably, the perovskite''s crystallinity is retained during these massive structural rearrangements.     

Photophysical Characteristics of Multicolor Emitting MDMO-PPV–DMP/ZnO Hybrid Nanocomposites

The tuning of photophysical properties of the poly[2-methoxy-5-(3,7-dimethyl-octyloxy)-1,4-phenylenevinylene]—end capped with dimethylphenyl (DMP), MDMO-PPV–DMP, was achieved by incorporation of ZnO NPs with various contents. Hybrid nanocomposites of MDMO-PPV–DMP with ZnO NPs were prepared by solution blending method and then deposited onto glass substrates. The structural properties of the hybrid nanocomposites samples were characterized using X-ray diffraction, FTIR, and FE-SEM, while their optical properties were extracted from the absorption and photoluminescence spectra. The energy band gap, energy tail, steepness parameter, and CIE chromatic coordinates were tuned by increase the content of ZnO NPs into the polymer matrix. The ZnO NPs incorporation assists the emission wavelength shift and multicolor emitting from the hybrid nanocomposites.     

Dependence of the Nanoscale Composite Morphology of Fe3O4 Nanoparticle-Infused Lysozyme Amyloid Fibrils on Timing of Infusion: A Combined SAXS and AFM Study

Understanding the formation process and the spatial distribution of nanoparticle (NP) clusters on amyloid fibrils is an essential step for the development of NP-based methods to inhibit aggregation of amyloidal proteins or reverse the assembling trend of the proto-fibrillary complexes that prompts pathogenesis of neuro degeneration. For this, a detailed structural determination of the diverse hybrid assemblies that are forming is needed, which can be achieved by advanced X-ray scattering techniques. Using a combined solution small angle X-ray scattering (SAXS) and atomic force microscopy (AFM) approach, this study investigates the intrinsic trends of the interaction between lysozyme amyloid fibrils (LAFs) and Fe₃O₄ NPs before and after fibrillization at nanometer resolution. AFM images reveal that the number of NP clusters interacting with the lysozyme fibers does not increase significantly with NP volume concentration, suggesting a saturation in NP aggregation on the fibrillary surface. The data indicate that the number of non-adsorbed Fe₃O₄ NPs is highly dependent on the timing of NP infusion within the synthesis process. SAXS data yield access to the spatial distribution, aggregation manner and density of NP clusters on the fibrillary surfaces. Employing modern data analysis approaches, the shape and internal structural morphology of the so formed nanocomposites are revealed. The combined experimental approach suggests that while Fe₃O₄ NPs infusion does not prevent the fibril-formation, the variation of NP concentration and size at different stages of the fibrillization process can impose a pronounced impact on the superficial and internal structural morphologies of these nanocomposites. These findings may be applicable in devising advanced therapeutic treatments for neurodegenerative diseases and designing novel bio-inorganic magnetic devices. Our results further demonstrate that modern X-ray methods give access to the structure of—and insight into the formation process of—biological–inorganic hybrid structures in solution.