Dynamic Light Scattering Data Research Articles

Alkanols Regulate the Fluidity of Phospholipid Bilayer in Accordance to Their Concentration and Polarity.

In spite of the widespread use of alkanols as penetration enhancers, their effect on vesicular formulations remains largely unexplored. These can affect the stability and integrity of the phospholipid bilayers. In this study, we have investigated the interaction of linear (ethanol, butanol, hexanol, octanol) and branched alkanols (t-amylol and t-butanol) with three phospholipids (soya lecithin, SL; soy L-α-phosphatidylcholine, SPC; and 1,2-dipalmitoyl-sn-glycero-3-phosphocholine, DPPC). Thermodynamic and structural aspects of these interactions were studied as a function of the alkanol concentration and chain length. Our interpretations are based on isothermal titration calorimetry (ITC) and dynamic light scattering (DLS) experiments. We observed one-site interactions wherein hydroxyl and acyl groups interacted with the polar and nonpolar regions of the phospholipid, respectively. The stability and structural integrity of bilayers appeared to be dependent upon (a) the hydrocarbon chain length and concentration of alcohols, and (b) the degree of unsaturation in the phospholipid molecule. We found that these interactions triggered a reduction in the enthalpy which was compensated by increased entropy, keeping free energy negative. Drop in enthalpy indicates reversible disordering of the bilayer which enables the diffusion of alcohol without triggering destabilization. Ethanol engaged predominantly with the interface, and it resulted in higher enthalpic changes. Interactions became increasingly unfavorable with longer alcohols - a cutoff point was recorded with hexanol. The overall sequence of membrane disordering capability was recorded as follows: ethanol < butanol < octanol < hexanol. Octanol's larger size restricted its penetration in the bilayer, and hence it caused less enthalpic changes relative to hexanol. This could also be verified from the trends in the area ratio of these vesicles obtained from the DLS data. Branched alkanols displayed a lower binding affinity with the phospholipids relative to their linear counterparts. These data are useful while contemplating the inclusion of short-chain alcohols as penetration enhancers in phospholipid vesicles.

Core-shell model of the clusters of CPEB4 isoforms preceding liquid-liquid phase separation

Protein solutions can undergo liquid-liquid phase separation (LLPS), where a dispersed phase with a low protein concentration coexists with coacervates with a high protein concentration. We focus on the low complexity N-terminal domain of cytoplasmic polyadenylation element binding-4 protein, CPEB4NTD, and its isoform depleted of the Exon4, CPEB4Δ4NTD. They both exhibit LLPS, but in contrast to most systems undergoing LLPS, the single-phase regime preceding LLPS consists mainly of soluble protein clusters. We combine experimental and theoretical approaches to resolve the internal structure of the clusters and the basis for their formation. Dynamic light scattering and atomic force microscopy show that both isoforms exhibit clusters with diameters ranging from 35 to 80 nm. Electron paramagnetic resonance spectroscopy of spin-labeled CPEB4NTD and CPEB4Δ4NTD revealed that these proteins have two distinct dynamical properties in both the clusters and coacervates. Based on the experimental results, we propose a core-shell structure for the clusters, which is supported by the agreement of the dynamic light scattering data on cluster size distribution with a statistical model developed to describe the structure of clusters. This model treats clusters as swollen micelles (microemulsions) where the core and the shell regions comprise different protein conformations, in agreement with the electron paramagnetic resonance detection of two protein populations. The effects of ionic strength and the addition of 1,6-hexanediol were used to probe the interactions responsible for cluster formation. While both CPEB4NTD and CPEB4Δ4NTD showed phase separation with increasing temperature and formed clusters, differences were found in the properties of the clusters and the coacervates. The data also suggested that the coacervates may consist of aggregates of clusters.

Abstract 3202: Investigating the induction of ferroptosis by nano drug delivery system

Abstract Prostate cancer is the second leading cause of cancer-related death in U.S. men. Genomic and clinical associations have identified loss of RB function as a dominant mechanism driving prostate cancer lethality. We recently demonstrated that ferroptosis induction in vivo by ferroptosis inducers blocks RB1-deficient prostate tumor growth and metastasis and leads to improved survival of the mice. As all ferroptosis inducers are newly discovered, there is a great need to improve their therapeutic potential through different avenues, including innovative drug delivery systems. Poly Lactic-co-glycolic acid (PLGA) is an FDA-approved biodegradable polymer. Due to their strong biocompatibility and consistent release, PLGA-based nanotherapeutics are an attractive carrier for small molecule drugs. This study aims to further improve the efficacy of ferroptosis induction against lethal RB1-deficient prostate cancer through PLGA-based ferroptosis-induced nanoparticles (NPs). The PLGA NPs encapsulating JKE-1674 were synthesized using the solvent evaporation method. The NPs were characterized using dynamic light scattering (DLS) and scanning electron microscopy (SEM) to assess the physicochemical properties of the NPs. The cell-killing efficacy of free-form or PLGA NP encapsulated JKE-1674 was then evaluated in vitro. Our analyses showed that the particle size and polydispersity index (PDI) of JKE-1674 PLGA NPs were 160.8 nm and 0.049, respectively. SEM images of JKE-1674 PLGA NPs further validated the DLS data. These findings suggest that encapsulation of JKE-1674 within the PLGA NPs results in a stable and biocompatible formation. Critically, JKE-1674 encapsulated by PLGA NPs is as potent as JKE-1674 in its free form to induce ferroptosis and associated lipid peroxidation in various human prostate cancer cell lines. This study presents the first effort to develop and validate PLGA-based ferroptosis-induced nanotherapeutics. Based on our in vitro data, we will test the in vivo efficacy of JKE-1674 PLGA NPs against lethal RB1 deficient prostate cancer. Citation Format: Eden M. Jacob, Sarah Y. Kim, Parul Sirohi, Mu-En Wang, Meredith L. Davis, Alyssa R. Bawcom, Ashutosh Chilkoti, Mark R. Wiesner, Jiaoti Huang, Ming Chen. Investigating the induction of ferroptosis by nano drug delivery system [abstract]. In: Proceedings of the American Association for Cancer Research Annual Meeting 2024; Part 1 (Regular Abstracts); 2024 Apr 5-10; San Diego, CA. Philadelphia (PA): AACR; Cancer Res 2024;84(6_Suppl):Abstract nr 3202.

Study of the molecular interaction of a phosphonium-based ionic liquid within myo-inositol and non-steroidal anti-inflammatory drugs.

Ionic liquids (ILs) can be used as carriers and solubilizers as well as for increasing the effectiveness of drugs. In the present investigation, the micellar properties of phosphonium-based ionic liquids (PILs) such as trihexyltetradecylphosphonium bis(2,4,4-trimethylpentyl)phosphinate ([P666(14)][THPP]) and the effect of carbocyclic sugar-based myo-inositol (MI) and non-steroidal anti-inflammatory drugs (NSAIDs), i.e. ibuprofen (IBU) or aspirin (ASP), on the PIL micellar system were studied using surface tension, conductivity, colorimetry, viscometry, FTIR, and dynamic light scattering (DLS) at a temperature of 299 ± 0.5 K. The critical micelle concentrations (CMCs), particle size, zeta potential, and various interfacial parameters were also included i.e., efficiency of adsorption (pC20), surface tension at CMC (γCMC), minimum surface area per molecule (Amin), surface pressure at CMC (πCMC), maximum surface excess concentration (Γmax), and various thermodynamic parameters, such as standard Gibbs free energy of adsorption , standard Gibbs free energy of micellization per alkyl tail , standard Gibbs free energy of the air-water interface (ΔG(s)min), standard Gibbs free energy of transfer , and standard Gibbs free energy of micellization . The adsorption and micellization characteristics became more spontaneous, as shown by the more negative values of and . Viscosity-based rheological properties were calculated for various PIL + MI and PIL + MI + NSAID systems. According to the DLS data, the PIL (Z = 316.4 nm) micellar system generates substantially bigger micelles in an aqueous solution of MI + ASP (Z = 801.7 nm) than in MI + IBU (Z = 674.7 nm). FTIR spectroscopy revealed the interactions of PIL with MI + ASP and MI + IBU, where it was observed that MI + IBU shows good agreement with the PIL system compared to MI + ASP. The current research will have effects on pharmaceutical sciences, molecular biology, and drug delivery.

Aggregation and Oligomerization Characterization of ß-Lactoglobulin Protein Using a Solid-State Nanopore Sensor.

Protein aggregation is linked to many chronic and devastating neurodegenerative human diseases and is strongly associated with aging. This work demonstrates that protein aggregation and oligomerization can be evaluated by a solid-state nanopore method at the single molecule level. A silicon nitride nanopore sensor was used to characterize both the amyloidogenic and native-state oligomerization of a model protein ß-lactoglobulin variant A (βLGa). The findings from the nanopore measurements are validated against atomic force microscopy (AFM) and dynamic light scattering (DLS) data, comparing βLGa aggregation from the same samples at various stages. By calibrating with linear and circular dsDNA, this study estimates the amyloid fibrils' length and diameter, the quantity of the βLGa aggregates, and their distribution. The nanopore results align with the DLS and AFM data and offer additional insight at the level of individual protein molecular assemblies. As a further demonstration of the nanopore technique, βLGa self-association and aggregation at pH 4.6 as a function of temperature were measured at high (2 M KCl) and low (0.1 M KCl) ionic strength. This research highlights the advantages and limitations of using solid-state nanopore methods for analyzing protein aggregation.

Structure and antiradical activity of N-monosubstituted amino acid derivatives of fullerene C60 in aqueous colloidal solutions

The dimensional characteristics of nanoparticles of N-mono- substituted amino acid derivatives of fullerene C60 (AAFDs) in aqueous colloidal solutions, determined by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS), were compared. The DLS data on the dimensional characteristics of fullerene C60 and AAFD nanoparticles, obtained at scattering angles of 90° and 173°, are close in values with a correlation coefficient of 0.89, and the SAXS data indicate that AAFDs form ordered structures in solution. Based on the results of DLS and the ability of fullerene and AAFDs to inhibit peroxyl radicals, it can be concluded that varying the concentrations of the studied compounds in the range from 10-7 to 10-3 m does not affect the degree of aggregation of their nanoparticles.

Amphoteric nano‐ and microgels with acrylamide backbone for potential application in oil recovery

AbstractAmphoteric nano‐ and microgels based on acrylamide (AAm), 3‐acrylamidopropyltrimethylammonium chloride (APTAC) and 2‐acrylamido‐2‐propanesulfonate sodium salt (AMPS) were prepared via inverse emulsion polymerization in the presence of crosslinking agent—N,N′‐methylenebisacrylamide (MBAA). Several polyampholyte nano‐ and microgel samples AAm‐APTAC‐AMPS with compositions (70:15:15, 80:10:10, and 90:5:5 mol%) were obtained and they were abbreviated as AAm70‐APTAC15‐AMPS15, AAm80‐APTAC10‐AMPS10 AAm90‐APTAC5‐AMPS5 (where the lower indexes indicate the molar concentration of monomers). The nano‐ and microgels were characterized by Fourier‐transform infrared spectroscopy, dynamic light scattering (DLS), transmission electron microscope (TEM), thermogravimetric analysis and interfacial tension measurements. The most attention was paid to the AAm80‐APTAC10‐AMPS10 microgel because its linear analog showed the best swelling capacity and the viscosifying effect for potential application in oil recovery. The influence of monomer concentration, surfactants, volume ratio of the water/organic phases, and the hydrophilic–lyophilic balance (HLB) on the average hydrodynamic size of the AAm80‐APTAC10‐AMPS10 nano‐ and microgels was studied. The size distribution of nano‐ and microgels derived from DLS data and TEM images was compared as a function of monomer concentration at constant surfactant concentration (6 wt%), HLB = 5.5 and mixture of water:oil = 60:40 vol%. Swelling of microgel particles in saline water due to the antipolyelectrolyte effect was observed. The applicability of amphoteric microgels AAm80‐APTAC10‐AMPS10 for oil recovery was tested on cores simulating the conditions of a model oil reservoir. The obtained results indicated that after the injection of around three pore volumes of the 2500 ppm microgel suspension into the sandstone core the permeability to brine decreased from 1.5 to 0.78 mD. For the first half of core sample the residual resistance factor was higher than the resistance factor, whereas for the second part of core sample these parameters were almost equal. Additional experiments with longer cores are needed to evaluate in‐depth propagation of microgels and permeability reduction in porous media.

Exploring the structural stability of hemoglobin in DBU-based ionic liquids: Insights from spectroscopic investigations

Globular proteins like heme proteins have garnered significant attention owing to their multiple applications in biochemical as well as biophysical processes and are the major functionalities in various pharmaceuticals and health care products. Hemoglobin (Hb), is the widely studied protein in existence and is the most familiar constituent of vertebrate erythrocytes. Protein solubility and stability in aqueous solutions is a major concern to develop therapeutic protein products as the protein lose its activity under unfolded state. Academic and industrial communities have shown great interest in the selection of an apt solvent for biomolecules in suitable biocatalytic applications. Ionic liquids (ILs) have emerged as a suitable cosolvent for the protein molecules by virtue of its high thermal as well as chemical stabilities. Each IL-Protein interaction is specific and generalizing the behaviour is tedious because the same IL can act as both stabilizer and denaturant depending on the external parameters and IL concentration as well. Here in this study, we have synthesized 1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU) based ILs derived from heterocyclic bases like 1,2,4- triazole, imidazole and morpholine. DBU based ILs are least explored in biomolecule applications but are known for their high thermal stabilities. The interaction of these ILs with hemoglobin was analysed using various spectroscopic techniques including UV–Visible spectroscopy, steady-state fluorescence, Fluorescence Time-Correlated Single Photon Counting (TCSPC), and Dynamic Light Scattering (DLS) to gain better insight into the effects of these ionic liquids on Hb. These results revealed that all the ILs used here are showing Hb friendly behaviour at lower concentrations as it retains the absorbance and fluorescence behaviour of the protein molecule. DLS data explains the solubilization of the Hb molecule, as the ‘z’ average values decreased with periodic addition of the ILs to the system. Quantitative evaluation of the Hb-IL interactions through Benesi-Hildebrand equation suggested that the possibility of complex formations are minimal and this further substantiate that these ILs can act as better cosolvents for Hb in various biochemical reactions.

Effects of model membranes on lysozyme amyloid aggregation.

The study of the interaction between lipid membranes and amyloidogenic peptides is a turning point for understanding the processes involving the cytotoxicity of peptides involved in neurodegenerative diseases. In this work, we perform an experimental study of model membrane-lysozyme interaction to understand how the formation of amyloid fibrils can be affected by the presence of polar and zwitterionic phospholipid molecules (1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine [POPC] and 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphoglycerol [POPG]). The study was conducted above and below the critical micellar concentration (CMC) using dynamic light scattering (DLS), atomic force microscopy (AFM), UV-Vis spectrophotometry, and the quartz crystal microbalance (QCM). Our results show that the presence of phospholipids appears to be a factor favoring the formation of amyloid aggregates. Spectrophotometric and DLS data revealed that the quantity of -structure increases in the presence of POPG and POPC at different concentrations. The presence of POPG and POPC increases the speed of the nucleation process, without altering the overall structures of the fibrillar final products.

Raynals, an online tool for the analysis of dynamic light scattering.

Dynamic light scattering (DLS) is routinely employed to assess the homogeneity and size-distribution profile of samples containing microscopic particles in suspension or solubilized polymers. In this work, Raynals, user-friendly software for the analysis of single-angle DLS data that uses the Tikhonov-Phillips regularization, is introduced. Its performance is evaluated on simulated and experimental data generated by different DLS instruments for several proteins and gold nanoparticles. DLS data can easily be misinterpreted and the simulation tools available in Raynals allow the limitations of the measurement and its resolution to be understood. It was designed as a tool to address the quality control of biological samples during sample preparation and optimization and it helps in the detection of aggregates, showing the influence of large particles. Lastly, Raynals provides flexibility in the way that the data are presented, allows the export of publication-quality figures, is free for academic use and can be accessed online on the eSPC data-analysis platform at https://spc.embl-hamburg.de/.

On the Fractionation and Physicochemical Characterisation of Self-Assembled Chitosan-DNA Polyelectrolyte Complexes.

Chitosan is extensively studied as a carrier for gene delivery and is an attractive non-viral gene vector owing to its polycationic, biodegradable, and biocompatible nature. Thus, it is essential to understand the chemistry of self-assembled chitosan-DNA complexation and their structural and functional properties, enabling the formation of an effective non-viral gene delivery system. In this study, two parent chitosans (samples NAS-032 and NAS-075; Mw range ~118-164 kDa) and their depolymerised derivatives (deploy nas-032 and deploy nas-075; Mw range 6-14 kDa) with degrees of acetylation 43.4 and 4.7%, respectively, were used to form polyelectrolyte complexes (PECs) with DNA at varying [-NH3+]/[-PO4-] (N/P) molar charge ratios. We investigated the formation of the PECs using ζ-potential, asymmetric flow field-flow fractionation (AF4) coupled with multiangle light scattering (MALS), refractive index (RI), ultraviolet (UV) and dynamic light scattering (DLS) detectors, and TEM imaging. PEC formation was confirmed by ζ-potential measurements that shifted from negative to positive values at N/P ratio ~2. The radius of gyration (Rg) was determined for the eluting fractions by AF4-MALS-RI-UV, while the corresponding hydrodynamic radius (Rh), by the DLS data. We studied the influence of different cross-flow rates on AF4 elution patterns for PECs obtained at N/P ratios 5, 10, and 20. The determined rho shape factor (ρ = Rg/Rh) values for the various PECs corresponded with a sphere morphology (ρ ~0.77-0.85), which was consistent with TEM images. The results of this study represent a further step towards the characterisation of chitosan-DNA PECs by the use of multi-detection AF4 as an important tool to fractionate and infer aspects of their morphology.

Investigating the effect of diluents and fat globules on the size measurement of casein micelles by dynamic light scattering

The hydrodynamic size of casein micelles was examined using dynamic light scattering (DLS). Four types of diluents [ultrafiltration (UF) permeate, lactose-free simulated milk ultrafiltrate (SMUF), calcium imidazole buffer, and deionised water] were compared in their effect on the stability of casein micelles. Results of dilution series and kinetic size measurements revealed that both UF permeate and lactose-free SMUF enable size measurements that are hardly affected by the required dilution step, whereas a calcium imidazole buffer containing 10 mm CaCl2 only could provide accurate sizing results within a short time after dilution. The contribution of residual fat globules to the particle size distribution was negligible in skim milk. For semi-skimmed milk, the size of the casein micelles could be estimated by subtracting the contribution of the fat droplets (obtained upon dilution in a casein dissolving solution) from the raw DLS data (as obtained upon dilution in milk ultrafiltrate).

Using sugars as both reducing and cryoprotectants of freeze-dried silver nanoparticles for improving long-term stability

This study has proposed using maltose and lactose as reducing and cryoprotectant agents to improve silver nanoparticles’ long-term stability (AgNPs). For the reducing performance, UV–vis spectroscopy revealed that both sugars could be used as reducing and eventually as capping agents of the as-synthesized AgNPs. For cryoprotective performance, the UV–vis spectroscopy and dynamic light scattering (DLS) showed that both sugars could prevent maltose-reduced (coded as AgNP-M) and lactose-reduced (coded as AgNP-L) AgNPs from irreversible aggregation under freezing and freeze-drying. For long-term stability, UV–vis spectroscopy, DLS, and transmission electron microscopy (TEM) data revealed that aged freeze-dried AgNP-M and AgNP-L were generally more stable than their non-freeze-dried counterparts under accelerated storage conditions. Likewise, the antibacterial and cytotoxic activities of aged freeze-dried AgNP-M and AgNP-L were close to those observed in their as-synthesized counterparts. Otherwise, aged non-freeze-dried AgNP-L demonstrated reduced antibacterial and cytotoxic activities, while such behavior was not present in the aged non-freeze-dried AgNP-M. These findings proved that maltose and lactose could emerge as a green alternative to synthesize AgNPs and simultaneously cryoprotect them during freezing and freeze-drying to achieve long-term stability.

Biosynthesis, Characterization, and Augmented Anticancer Activity of ZrO2 Doped ZnO/rGO Nanocomposite.

Fabrication of ZnO nanoparticles (NPs) via green process has received enormous attention for its application in biomedicine. Here, a simple and cost-effective green route is reported for the synthesis of ZrO2-doped ZnO/reduced graphene oxide nanocomposites (ZnO/ZrO2/rGO NCs) exploiting ginger rhizome extract. Our aim was to improve the anticancer performance of ZnO/ZrO2/rGO NCs without toxicity to normal cells. The preparation of pure ZnO NPs, ZnO/ZrO2 NCs, and ZnO/ZrO2/rGO NCs was confirmed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), photoluminescence (PL), and dynamic light scattering (DLS). XRD spectra of ZnO/ZrO2/rGO NCs exhibited two distinct sets of diffraction peaks, ZnO wurtzite structure, and ZrO2 phases (monoclinic + tetragonal). The SEM and TEM data show that ZrO2-doped ZnO particles were uniformly distributed on rGO sheets with the excellent quality of lattice fringes without alterations. PL spectra intensity and particle size of ZnO decreased after ZrO2-doping and rGO addition. DLS data demonstrated that green prepared samples show excellent colloidal stability in aqueous suspension. Biological results showed that ZnO/ZrO2/rGO NCs display around 3.5-fold higher anticancer efficacy in human lung cancer (A549) and breast cancer (MCF7) cells than ZnO NPs. A mechanistic approach suggested that the anticancer response of ZnO/ZrO2/rGO NCs was mediated via oxidative stress evident by the induction of the intracellular reactive oxygen species level and the reduction of the glutathione level. Moreover, green prepared nanostructures display good cytocompatibility in normal cell lines; human lung fibroblasts (IMR90) and breast epithelial (MCF10A) cells. However, the cytocompatibility of ZnO/ZrO2/rGO NCs in normal cells was better than those of pure ZnO NPs and ZnO/ZrO2 NCs. Augmented anticancer potential and improved cytocompatibility of ZnO/ZrO2/rGO NCs was due to ginger extract mediated beneficial synergism between ZnO, ZrO2, and rGO. This novel investigation emphasizes the significance of medicinal herb mediated ZnO-based NCs synthesis for biomedical research.

Double Stimuli-Responsive di- and Triblock Copolymers of Poly(N-isopropylacrylamide) and Poly(1-vinylimidazole): Synthesis and Self-Assembly.

For the first time, double stimuli-responsive properties of poly(N-isopropylacrylamide) (PNIPA) and poly(1-vinylimidazole) (PVIM) block copolymers in aqueous solutions were studied. The synthesis of PNIPA60-b-PVIM90 and PNIPA28-b-PVIM62-b-PNIPA29 was performed using reversible addition-fragmentation chain transfer (RAFT) polymerization. The polymers were characterized by size exclusion chromatography and 1H NMR spectroscopy. The conformational behavior of the polymers was studied using dynamic light scattering (DLS) and fluorescence spectroscopy (FS). It was found that PNIPA and block copolymers conformation and ability for self-assembly in aqueous medium below and above cloud point temperature depend on the locus of hydrophobic groups derived from the RAFT agent within the chain. Additionally, the length of PVIM block, its locus in the chain and charge perform an important role in the stabilization of macromolecular micelles and aggregates below and above cloud point temperature. At 25 °C the average hydrodynamic radius (Rh) of the block copolymer particles at pH 3 is lower than at pH 9 implying the self-assembling of macromolecules in the latter case. Cloud points of PNIPA60-b-PVIM90 are ~43 °C and ~37 °C at a pH of 3 and 9 and of PNIPA28-b-PVIM62-b-PNIPA29 they are ~35 °C and 31 °C at a pH of 3 and 9. Around cloud point independently of pH, the Rh value for triblock copolymer rises sharply, achieves the maximum value, then falls and reaches the constant value, while for diblock copolymer, it steadily grows after reaching cloud point. The information about polarity of microenvironment around polymer obtained by FS accords with DLS data.

Dynamic light scattering and transmission electron microscopy in drug delivery: a roadmap for correct characterization of nanoparticles and interpretation of results.

In this focus article, we provide a scrutinizing analysis of transmission electron microscopy (TEM) and dynamic light scattering (DLS) as the two common methods to study the sizes of nanoparticles with focus on the application in pharmaceutics and drug delivery. Control over the size and shape of nanoparticles is one of the key factors for many biomedical systems. Particle size will substantially affect their permeation through biological membranes. For example, an enhanced permeation and retention effect requires a very narrow range of sizes of nanoparticles (50-200 nm) and even a minor deviation from these values will substantially affect the delivery of drug nanocarriers to the tumour. However, amazingly a great number of research papers in pharmaceutics and drug delivery report a striking difference in nanoparticle size measured by the two most popular experimental techniques (TEM and DLS). In some cases, this difference was reported to be 200-300%, raising the question of which size measurement result is more trustworthy. In this focus article, we primarily focus on the physical aspects that are responsible for the routinely observed mismatch between TEM and DLS results. Some of these factors such as concentration and angle dependencies are commonly underestimated and misinterpreted. We convincingly show that correctly used experimental procedures and a thorough analysis of results generated using both methods can eliminate the DLS and TEM data mismatch completely or will make the results much closer to each other. Also, we provide a clear roadmap for drug delivery and pharmaceutical researchers to conduct reliable DLS measurements.

Synthesis and Characterization of Polypyrrole/Fe3O4 Nanocomposites: A Promising Material Against Carbon Steel Corrosion

The use of conducting polymers as coating layers for the protection of surfaces against corrosion represents an important topic for investigation, as reported in the literature. In this work, polypyrrole/Fe3O4 nanoparticles (Fe3O4_NPs/PPy) hybrid nanocomposites (HN) were incorporated as anticorrosive additives in an epoxy paint to protect SAE 1010 carbon steel from corrosion. The HN particles were obtained by chemical polymerization of pyrrole in an aqueous solution in the presence of Fe3O4_NPs and were characterized by infrared absorption spectrophotometry, dynamic light scattering (DLS), X-ray diffraction (XRD), transmission electron microscopy (TEM). The electrochemical impedance spectroscopy (EIS) was used in the analysis of the electrochemical response of the coated surface with and without HN. DLS data showed that the Fe3O4_NPs and Fe3O4_NPs/PPy obtained in solution present average diameters of (19.7 ± 9.6) nm and (63.5 ± 27.7) nm, respectively. TEM images showed Fe3O4_NPs with smaller sizes (10 nm - 30 nm), and that the HN had diameters smaller than 100 nm, consisting of Fe3O4 cores coated with polypyrrole. EIS measurements have shown that the addition of HN to the epoxy paint could improve the efficiency of the anticorrosive coating when compared to the original epoxy paint prepared without any corrosion inhibitor.

Cellulose nanocrystals from Siam weed: Synthesis and physicochemical characterization

The use of biomass for the development of environmentally friendly and industrially useful materials is still attracting global interest. Herein, cellulose nanocrystals were prepared from Siam weed. The production steps involved dewaxing the biomass sample, bleaching treatment, alkali treatment and acid hydrolysis. The resulting cellulose nanocrystals were characterized using Fourier transformed infrared (FTIR) spectroscopy, X-ray diffraction (XRD) spectroscopy, thermo-gravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and dynamic light scattering (DLS) technique. Chemical composition results showed that Siam weed contained 39.6% cellulose, 27.5% hemicellulose, 28.7% lignin and 4.2% extractive. FTIR spectrum confirmed the presence of cellulose and absence of lignin and hemicellulose while XRD analysis revealed that the cellulose nanocrystals have crystallinity index of 66.2% and particle size of 2.2 nm. TGA revealed that thermal stability of raw Siam weed is lower than that of its cellulose nanocrystals due to the presence of the non-cellulosic component with lower temperature of degradation. SEM revealed that degradation of cellulosic chain had occurred. TEM confirmed that the crystal size is in the nanoscale with an average size <100 nm. DLS data revealed a nanocellulose with an average hydrodynamic size of 213 nm and a zeta potential at −9.57 mV.

Colloidal and Sedimentation Behavior of Kaolinite Suspension in Presence of Non-Ionic Polyacrylamide (PAM).

Colloidal behavior of kaolinite particles in water was investigated in this manuscript, without and with the addition of a polymer flocculant (non-anionic polyacrylamide (PAM)), using diverse imaging techniques in addition to LUMisizer. The addition of PAM was found to be causing the formation of bridges among particles thus increasing their settling rates to the bottom of the container. To assess the size of flocs and the potential morphology of PAM around particles and their clusters, the state of flocs formation and polymer distribution was analyzed through various microscopical techniques, namely scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM and TEM results revealed that, in the absence of PAM, the floc structure of the sediment was loose and irregularly distributed, while the presence of PAM made the sediment structures greatly denser. Later, using LUMisizer, dynamic light scattering (DLS) and the zeta potential of kaolinite, sedimentation, and colloidal behavior of suspension came under scrutiny. Using LUMisizer, the maximum packing and settling rates of the particles were experimentally obtained as roughly 44 vol%; settling rates were estimated in 63-352 µm/s when centrifugal force varied and, using maximum packing values, compressive yield was estimated to vary between 48-94 kPa. The results of this study are instructive in choosing appropriate polymers and operating conditions to settle clay minerals in tailing ponds. Additionally, the maximum packing of kaolinite particles was simulated with spherical particles with varied polydispersity to connect DLS data to the maximum packing values obtained using LUMisizer; the little discrepancy between simulation and experimental values was found to be encouraging.

Effects of Molecular Crowding and Betaine on HSPB5 Interactions, with Target Proteins Differing in the Quaternary Structure and Aggregation Mechanism

The aggregation of intracellular proteins may be enhanced under stress. The expression of heat-shock proteins (HSPs) and the accumulation of osmolytes are among the cellular protective mechanisms in these conditions. In addition, one should remember that the cell environment is highly crowded. The antiaggregation activity of HSPB5 and the effect on it of either a crowding agent (polyethylene glycol (PEG)) or an osmolyte (betaine), or their mixture, were tested on the aggregation of two target proteins that differ in the order of aggregation with respect to the protein: thermal aggregation of glutamate dehydrogenase and DTT-induced aggregation of lysozyme. The kinetic analysis of the dynamic light-scattering data indicates that crowding can decrease the chaperone-like activity of HSPB5. Nonetheless, the analytical ultracentrifugation shows the protective effect of HSPB5, which retains protein aggregates in a soluble state. Overall, various additives may either improve or impair the antiaggregation activity of HSPB5 against different protein targets. The mixed crowding arising from the presence of PEG and 1 M betaine demonstrates an extraordinary effect on the oligomeric state of protein aggregates. The shift in the equilibrium of HSPB5 dynamic ensembles allows for the regulation of its antiaggregation activity. Crowding can modulate HSPB5 activity by affecting protein-protein interactions.