Synthesis and Study of Thermoresponsive Amphiphilic Copolymers via RAFT Polymerization

Synthesis and study of well-defined thermoresponsive amphiphilic copolymers with various compositions were reported. Kinetics of the reversible addition-fragmentation chain transfer (RAFT) (co)polymerization of styrene (St) and oligo(ethylene glycol) methyl ether methacrylate (PEO5MEMA) was studied by size exclusion chromatography (SEC) and 1H NMR spectroscopy, which allows calculating not only (co)polymerization parameters but also gives valuable information on RAFT (co)polymerization kinetics, process control, and chain propagation. Molecular weight Mn and dispersity Đ of the copolymers were determined by SEC with triple detection. The detailed investigation of styrene and PEO5MEMA (co)polymerization showed that both monomers prefer cross-polymerization due to their low reactivity ratios (r1 < 1, r2 < 1); therefore, the distribution of monomeric units across the copolymer chain of p(St-co-PEO5MEMA) with various compositions is almost ideally statistical or azeotropic. The thermoresponsive properties of p(St-co-PEO5MEMA) copolymers in aqueous solutions as a function of different hydrophilic/hydrophobic substituent ratios were evaluated by measuring the changes in hydrodynamic parameters under applied temperature using the dynamic light scattering method (DLS).

Study of colloidal gold nanorods in liquid dispersions using light scattering methods

Five samples of liquid dispersions of colloidal gold nanorods having various aspect ratios have been studied using light scattering methods. Transmission electron microscopy has been employed as a reference method. Advantages and drawbacks of dynamic light scattering and nanoparticle tracking analysis methods for study of nanoparticle geometrical parameters and concentration, sample monodispersity degree and detection of large particle aggregations and quasispherical impurities have been demonstrated. We show that depolarized dynamic light scattering method can be used for analysis of geometrical parameters of colloidal gold nanorods in liquid dispersions. The measurement results depend largely on the presence of large impurity particles or particle aggregations in samples. In turn the presence of large particles in dispersions can be detected using dynamic light scattering methods or nanoparticle tracking analysis. Dynamic light scattering method is more sensitive to the presence of even small quantities of large impurities or aggregations in samples. The monodispersity degree of nanorod liquid dispersions can also be assessed using dynamic light scattering and nanoparticle tracking analysis methods, and the measurement results can be considered more statistically significant in comparison with electron microscopy because a larger number of particles are analyzed. An increase in the concentration of spherical particles in compound dispersions of colloidal gold nanospheres and nanorods leads to a decrease in the contribution of the rotational mode to the overall scattering intensity. Data on the concentration of quasispherical impurities in samples of colloidal gold nanorod liquid dispersions have been reported on the basis of scattered light depolarization degree measurements.

Bio-Catalytic Activity of Novel Mentha arvensis Intervened Biocompatible Magnesium Oxide Nanomaterials

In the present study Mentha arvensis medaited Magnesium oxide nanoparticles were synthesized by novel green route followed by advanced characterization via XRD, FTIR, UV, SEM, TEM, DLS and TGA. The mean grain size of 32.4 nm and crystallite fcc morphology were confirmed by X-ray diffractive analysis. Scanning and Transmission electron microscopy analysis revealed the spherical and elliptical morphologies of the biosynthesized nanoparticles. Particle surface charge of −16.1 mV were determined by zeta potential and zeta size of 30–120 nm via dynamic light scattering method. Fourier transform spectroscopic analysis revealed the possible involvement of functional groups in the plant extract in reduction of Mg2+ ions to Mg0. Furthermore, the antioxidant, anti-Alzheimer, anti-cancer, and anti-H. pylori activities were performed. The results revealed that MgO-NPs has significant anti-H. pyloric potential by giving ZOI of 17.19 ± 0.83 mm against Helicobacter felis followed by Helicobacter suis. MgO-NPs inhibited protein kinase enzyme up to 12.44 ± 0.72% at 5 mg/mL and thus showed eminent anticancer activity. Significant free radicals scavenging and hemocompatability was also shown by MgO-NPs. MgO-NPs also displayed good inhibition potential against Hela cell lines with maximum inhibition of 49.49 ± 1.18 at 400 µg/mL. Owing to ecofriendly synthesis, non-toxic and biocompatible nature, Mentha arvensis synthesized MgO-NPs can be used as potent antimicrobial agent in therapeutic applications.

Influence of Activators and Inhibitors on the Collagenase with Collagen Interaction Monitored by Dynamic Light Scattering in Solutions

Real–time digestion of type I collagen molecules by bacterial collagenase from Clostridium histolyticum has been monitored using Dynamic Light Scattering method. Time dependencies for translation diffusion coefficient (Dt) and hydrodynamic radius (RH) on were obtained for pure “collagen + collagenase” Tris–HCl buffer solution at different temperatures and for solutions with added CaCl2, ZnCl2 and MgCl2 and EDTA. It was shown that digestion of type I collagen molecules by bacterial collagenase is the first-order reaction. Reaction rate coefficients were calculated.

PECULARITIES OF MICELLE FORMATION OF PENTACYCLIC GLYCOSIDES IN AQUEOUS SOLUTIONS

The regularities of changes in structural characteristics during the formation of associates in micellar aqueous solutions of triterpene saponins Quillaja Saponin and Sapindus Mukorossi are considered. The dependence of surface tension and adsorption on the concentration of an aqueous saponin solution is analyzed, and the values of surface activity and parameters of the adsorption layer are calculated. The average values of diffusion coefficients for spherical and cylindrical micelles are determined based on the measurement of the solution viscosity. The effect of the electrolyte solution on the surface tension and viscosity of glycoside solutions is studied: when the electrolyte is introduced into the saponin solution, the surface tension decreases, which leads to a shift in the critical concentration of micelle formation towards lower concentrations. The introduction of potassium chloride electrolyte reduces the degree of ionization and, as a result of suppressing the electroviscosity effect, leads to a decrease in the viscosity of the solution. The dynamic light scattering method is used to determine the size of glycoside aggregates. It is established that there are aggregates of several sizes in an aqueous solution of saponin. The size and shape of aggregates were calculated using the concepts of micelle packing parameters. In the region of very low concentrations of glycoside solutions, when approaching the critical concentration of micelle formation in the solution, there are spherical micelles. A further increase in the saponin concentration in the solution leads to a decrease in the content of structures with a hydrodynamic radius of 50-80 nm and the appearance of larger agglomerates with sizes greater than 100 nm. It was found that micelles acquire a less hydrated and more densely packed cylindrical shape in the concentration range of 1.7-2.6 mmol/dm3. Compaction of associates leads to an increase in the content of particles with a hydrodynamic radius of 150-250 nm and larger ones, and their presence predicts the appearance of larger agglomerates. Analyzing the data obtained using the dynamic light scattering method, it can be concluded that aggregates of several sizes co-exist in the volume of aqueous saponin solutions at certain concentrations.

Structural Changes of the Lipid Model Systems in the Presence of Enzymes or Silver Nanoparticles

This work aimed to study the interaction of silver nanoparticles (AgNP) and lipases with models of biological membranes based on natural phospholipid and cholesterol. The crude phosphatidylcholine from egg yolk (PCe1) and synthetic cholesterol (Chol) were obtained from Sigma-Aldrich. Porcine pancreatic lipase (PPL) was obtained by purification from the hog pancreas. AgNP dispersion was prepared by the well-known citrate method. Measurement of surface tension (ST) was carried out using a BPA-1P device. The equilibrium surface tension (eST) was obtained by calculating the ST-time isotherms using the ADSA program. The particle sizes were determined by the dynamic light scattering method. An addition of AgNPs led to a pronounced decrease in both ST and eST (whereas almost no changes occurred by lipase addition), and AgNPs destructed the large lipid particles. The average lipid particle diameter values changed drastically, whereas the effective particle diameter values were almost the same by lipase addition. Thus, the interactions of AgNPs or lipase with the mixture of natural phospholipid and cholesterol have had entirely different features. These effects are interesting for modeling the interactions of inorganic and organic compounds with biological membranes.

Synergic Effect of Selected Ingredients and Calcium Chloride on the Technological, Molecular and Microbial Usefulness of Eggshells and Their Impact on Sensory Properties in a Food Model System

Lower levels of calcium in adults increase the risk for osteoporosis, and in children, low calcium levels can impact their potential adult height. The study objective was to analyze the bioavailability and physicochemical properties of a calcium preparation based on chicken eggs. The base calcium preparation was enriched with one of a variety of biologically active substances, inter alia, vitamin D3, vitamin K, lysine, lactose, magnesium chloride and inulin. The newly developed calcium preparations were subjected to structural analysis using X-ray diffraction and scanning electron microscopy, and the hydrodynamic diameter for the molecules was determined using the dynamic light scattering method and their zeta potential. To determine the optimum storage conditions of calcium preparations, their hygroscopicity and bulk density were determined. The calcium preparations were also added to selected food products, such as apple juice with mango, fruit dessert (jelly) and beef meatballs. The enriched food products were subjected to sensory analysis. The study demonstrated the significant influence of additives to calcium preparation in terms of its hygroscopicity and morphology. It was found that all products with the addition of analyzed preparations were characterized by high sensory desirability. The results presented in the study comprise the basis for the development of new food products, enriched with calcium.

Study of gold nanoparticles’ preparation through ultrasonic spray pyrolysis and lyophilisation for possible use as markers in LFIA tests

To monitor the progress and prevent the spread of the COVID-19 pandemic in real time and outside laboratories, it is essential to develop effective tests that can ensure rapid, selective, and reliable diagnosis of infected persons in different environments. Key in this regard is the lateral flow immunoassays (LFIAs) that can detect the presence of the SARS-CoV-2 virus quickly, with the aid of nanoparticles (NPs) and specific proteins. We report the use of gold (Au) NPs AuNPs synthesised from a gold(iii) chloride tetrahydrate precursor in a USP device and collected in a suspension composed of deionised water with polyvinylpyrrolidone as a stabiliser and cryoprotectant. In combination with freeze-drying of the AuNPs’ suspension to achieve water elimination, improved stability, and the target concentration, they exhibit the necessary properties for use as markers in LFIA rapid diagnostic tests. This was confirmed by complementary characterisation determined by using the techniques including inductively coupled plasma-optical emission spectrometry, dynamic light scattering method and zeta-potential, ultraviolet-visible spectroscopy, X-ray diffraction, scanning electron microscopy with energy dispersion spectrometer, and transmission electron microscopy, as well as with the preparation of a prototype LFIA test strip with AuNPs. Thus, such AuNPs, as well as the USP method, show promise for the development of new markers for use in LFIA.

Analysis of NMR Spectra of Submicro-Containers with Biocide DCOIT

Nowadays, the search for and development of new forms of materials with biocides is an actual problem of the modern science of nanosized materials due to the problem of microbiological contamination, which can be solved by using nanocontainers carrying biocides. Depending on the morphology of the nanocontainers and the filled active agents, it is possible to create coatings with specially designed self-healing functionality or multifunctional properties. The purpose of this work was to produce submicro-containers (SMCs) with a shell of SiO2 nanoparticles and a core of polymerized 3-(trimethoxysilyl) propyl methacrylate filled with 5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) in an oil in water (O/W) emulsion. The chemical nature of the individual components of the system and nano-capsules were investigated using NMR spectroscopy. The size and zeta potential of the SMCs were measured by a dynamic light scattering method (d = 170–180 nm, polydispersity index PDI = 0.125 and zeta-potential = 55 mV), the morphology of their outer surface was determined using SEM. The results of NMR analysis showed that during the addition of the biocide into the SMCs, its chemical structure is retained, as is its activity. Minor changes in the chemical shifts of the 1H NMR spectra of the SMCs with DCOIT, as well as of the biocide itself, confirm the inclusion of DCOIT inside the SMCs.

Research of the oils for ship engine by means of dynamic light scattering method

В данной статье исследована возможность использования метода фотонной корреляционной спектроскопии с целью диагностики судовых двигателей по отработанному моторному маслу для повышения экономичности и безопасности эксплуатации морских судов. Необходимость разработки и внедрения новых эффективных методов диагностики судовых дизелей является актуальной задачей. Целью данной работы явилось исследование ряда свежих и отработанных масел методом динамического рассеяния света для определения изменений, происходящих с маслом в процессе эксплуатации судового дизеля, и выяснения связи этих изменений с неисправностями двигателя. В литературе публикации о подобных исследованиях отсутствуют и результаты, приводимые в настоящей работе, обладают новизной. При исследовании использовался метод фотонной корреляционной спектроскопии для измерения корреляционных функций и последующего получения распределений времен корреляции, коэффициентов диффузии и размеров частиц. Для инверсии преобразования Лапласа применялся метод, основанный на минимизации среднеквадратичного отклонения и регуляризации (RILT), модифицированный для нахождения распределения времен корреляции. Установлено, что распределения гидродинамических радиусов частиц для свежих и отработанных масел существенно различаются. По характеру распределений крупных частиц установлено, что в отработанных маслах понижается уровень агрегации или мицеллообразования полимера модификатора вязкости. Показано, что метод динамического рассеяния света позволяет получать параметры, пригодные для анализа состояния моторного масла и для получения диагностических данных о состоянии двигателя по отработанному маслу. Полученные результаты обладают надежностью, что подтверждается многократной апробацией и общим признанием эффективности метода фотонной корреляционной спектроскопии в разных областях науки. Достоверность полученных результатов подтверждается устойчивостью экспериментов при их многократном повторении, корректностью математической обработки и широкой апробацией используемых методов в мировой практике. Тhe possibility of using the photon correlation spectroscopy method for the purpose of diagnostics of marine engines based on used engine oil to improve the efficiency and safety of operation of marine vessels is investigated in this article. The need to develop and implement new effective methods of diagnostics of marine diesel engines is an actual task. The purpose of this work was to study a number of fresh and used oils by dynamic light scattering method to determine the changes that occur with the oil during the operation of a marine diesel engine, and to find out the connection of these changes with engine failures. There are no publications about such studies in the literature, and the results presented in this paper are new. The photon correlation spectroscopy method was used to measure correlation functions and then obtain distributions of correlation times, diffusion coefficients, and particle sizes. To invert the Laplace transform, we used a method based on minimizing the standard deviation and regularization (RILT), modified to find the correlation time distribution. It was found that the distributions of hydrodynamic radii of particles for fresh and used oils differ significantly. By the character of the distributions of large particles, it was found that the level of aggregation or micelle formation of the polymer of the viscosity modifier decreases in the used oils. It is shown that the dynamic light scattering method allows to obtain parameters suitable for analyzing the state of engine oil and for obtaining diagnostic data on the state of the engine for used oil. The results obtained are reliable, which is confirmed by repeated testing and general recognition of the effectiveness of the photon correlation spectroscopy method in various fields of science. The reliability of the results obtained is confirmed by the stability of experiments when repeated many times, the correctness of mathematical processing and wide approbation of the methods used in the world practice.