Solubility–spinnability map and model for the preparation of fibres of polyethylene (terephthalate) using gyration and pressure

AbstractThe selection of a solvent or a solvent system is a fundamental and a crucial step in spinning fibres using a selected process. Solvent selection determines the critical minimum polymer concentration and the critical minimum chain entanglement which allows the spinning of nanofibres rather than other hybrid morphologies such as beaded structures. Pressurised gyration, which simultaneously combines the use of gas pressure and rotation, is used as the processing and forming route for spinning fibres in this work. This study investigates 23 different solvents and solvent systems spread on a wide area of a Teas graph and able to dissolve the functional polymer polyethylene (terephthalate) (PET) and spin products by the application of pressurised gyration. The results are mapped on a Teas graph to identify the solubility–spinnability region. Based on this solubility–spinnability region, various solvents and binary solvent systems that allow the making of PET fibres are suggested. Scaling laws for the relationship between polymer concentration and specific viscosity are identified. The structural evolution in the fibres prepared is elucidated. For the first time, a mathematical model to scale fibre diameter with respect to flow properties and processing parameters encountered in pressurised gyration has been successfully developed

pH Alteration in Plant-Mediated Green Synthesis and Its Resultant Impact on Antimicrobial Properties of Silver Nanoparticles (AgNPs)

© 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/)Plant-mediated green synthesis is a cost-effective and eco-friendly process used to synthesize metallic nanoparticles. Experimental pH is of interest due to its ability to influence nanoparticle size and shape; however, little has been explored in comparison to the influence of this parameter on the therapeutic potential of resultant metallic nanoparticles. Our work investigated the influence of pH alternation on antimicrobial properties of plant-mediated green synthesized (using Spinacia oleracea leaf extract) silver nanoparticles. We further investigated if the antimicrobial activity was sustained at 8 weeks (after initial green synthesis). Antimicrobial properties were evaluated against Escherichia coli, Staphylococcus aureus, and Candida albicans. Our work confirmed that experimental pH in plant-mediated green synthesis of silver nanoparticles influenced their resultant antimicrobial properties. Silver nanoparticles generated at experimental pH 4.5, and nine showed activity against E. coli which was sustained at various levels over 8 weeks. No antimicrobial activity was observed against S. aureus, and weak antimicrobial activity against C. albicans. These interesting findings highlight the importance of experimental pH. Further understanding of the role experimental pH plays on resultant metallic nanoparticle properties as it relates to biological and therapeutic impact is required, which will have an impact on wider applications beyond antimicrobial activity.Peer reviewe

Mucoadhesion of Progesterone-Loaded Drug Delivery Nanofiber Constructs

Mucoadhesive delivery systems have attracted remarkable interest recently, especially for their potential to prolong dosage form resident times at sites of application such as the vagina or nasal cavity, thereby improving convenience and compliance as a result of less frequent dosage. Mucoadhesive capabilities need to be routinely quantified during the development of these systems. This is however logistically challenging due to difficulties in obtaining and preparing viable mucosa tissues for experiments. Utilizing artificial membranes as a suitable alternative for quicker and easier analyses of mucoadhesion of these systems is currently being explored. In this study, the mucoadhesive interactions between progesterone-loaded fibers (with varying carboxymethyl cellulose (CMC) content) and either artificial (cellulose acetate) or mucosa membranes are investigated by texture analysis and results across models are compared. Mucoadhesion to artificial membrane was about 10 times that of mucosa, though statistically significant (p = 0.027) association between the 2 data sets was observed. Furthermore, a hypothesis relating fiber–mucosa interfacial roughness (and unfilled void spaces on mucosa) to mucoadhesion, deduced from some classical mucoadhesion theories, was tested to determine its validity. Points of interaction between the fiber and mucosa membrane were examined using atomic force microscopy (AFM) to determine the depths of interpenetration and unfilled voids/roughness, features crucial to mucoadhesion according to the diffusion and mechanical theories of mucoadhesion. A Kendall’s tau and Goodman–Kruskal’s gamma tests established a monotonic relationship between detaching forces and roughness, significant with p-values of 0.014 and 0.027, respectively. A similar relationship between CMC concentration and interfacial roughness was also confirmed. We conclude that AFM analysis of surface geometry following mucoadhesion can be explored for quantifying mucoadhesion as data from interfacial images correlates significantly with corresponding detaching forces, a well-established function of mucoadhesion

The development of progesterone-loaded nanofibers using pressurized gyration: A novel approach to vaginal delivery for the prevention of pre-term birth

Recent evidence has continued to support the applicability of progesterone in preventing preterm birth, hence the development of an appropriate vaginal delivery system for this drug would be of considerable interest. Here, we describe the development of progesterone-loaded bioadhesive nanofibers using pressurized gyration for potential incorporation into a vaginal insert, with a particular view to addressing the challenges of incorporating a poorly water-soluble drug into a hydrophilic nanofiber carrier. Polyethylene oxide and carboxymethyl cellulose were chosen as polymers to develop the carrier systems, based on previous evidence of their yielding mucoadhesive nanofibers using the pressurized gyration technique. The fabrication parameters such as solvent system, initial drug loading and polymer composition were varied to facilitate optimisation of fiber structure and efficiency of drug incorporation. Such studies resulted in the formation of nanofibers with satisfactory surface appearance, diameters in the region of 400 nm and loading of up to 25% progesterone. Thermal and spectroscopic analyses indicated that the drug was incorporated in a nanocrystalline state. Release from the drug-loaded fibers indicated comparable rates of progesterone dissolution to that of Cyclogest, a commercially available progesterone pessary, allowing release over a period of hours. Overall, the study has shown that pressurized gyration may produce bioadhesive progesterone-loaded nanofibers which have satisfactory loading of a poorly water-soluble drug as well as having suitable structural and release properties. The technique is also capable of producing fibers at a yield commensurate with practical applicability, hence we believe that the approach shows considerable promise for the development of progesterone dosage forms for vaginal application

Making nanofibres of mucoadhesive polymer blends for vaginal therapies

Nanofibres from mucoadhesive polymers could combine their material properties with unique structural characteristics for superior drug delivery performance. However, due to their chain structure a significant proportion of mucoadhesive polymers such as polysaccharides cannot be easily spun into fibres. In this study, we demonstrate the possibility of using polymer blends for the preparation of nanofibres that offer substantial mucoadhesive capabilities. Fibres from four different polymers were obtained by pressurised gyration at different working pressures and a rotation speed of 24,000 rpm. Electron microscopy indicates that structurally well-defined fibres with diameters from less than 100 nm upwards were successfully produced. Quantitative relationships between the physical properties and fibre characteristics were established while the fibre compositions were confirmed to contain features likely to confer mucoadhesive properties. Finally, a combination of texture analysis and atomic force microscopy was used to verify the benefit of transforming polymer powders into nanofibre structures, as far as mucoadhesive potential is concerned

Thermal Behavior of Benzoic Acid/Isonicotinamide Binary Cocrystals

YesA comprehensive study of the thermal behavior of the 1:1 and 2:1 benzoic acid/isonicotinamide cocrystals is reported. The 1:1 material shows a simple unit cell expansion followed by melting upon heating. The 2:1 crystal exhibits more complex behavior. Its unit cell first expands upon heating, as a result of C–H···π interactions being lengthened. It then is converted into the 1:1 crystal, as demonstrated by significant changes in its X-ray diffraction pattern. The loss of 1 equiv of benzoic acid is confirmed by thermogravimetric analysis–mass spectrometry. Hot stage microscopy confirms that, as intuitively expected, the transformation begins at the crystal surface. The temperature at which conversion occurs is highly dependent on the sample mass and geometry, being reduced when the sample is under a gas flow or has a greater exposed surface area but increased when the heating rate is elevated

Development of micro-fibrous solid dispersions of poorly water-soluble drugs in sucrose using temperature-controlled centrifugal spinning

Solid dispersion technology represents a successful approach to addressing the bioavailability issues caused by the low aqueous solubility of many Biopharmaceutics Classification System (BCS) Class II drugs. In this study, the use of high-yield manufacture of fiber-based dispersion is explored as an alternative approach to monolith production methods. A temperature-controlled solvent-free centrifugal spinning process was used to produce sucrose-based microfibers containing the poorly water-soluble drugs olanzapine and piroxicam (both BCS Class II); these were successfully incorporated into the microfibers and the basic characteristics of fiber diameter, glassy behavior, drug loading capacity and drug-sucrose interaction assessment were measured. Scanning electron microscopy revealed that bead-free drug-loaded microfibers with homogenous morphology and diameter in the range of a few micrometers were prepared using our process. Differential scanning calorimetric and X-ray diffraction analyses showed that both drug and carrier were present in the amorphous state in the microfibers, although in the case of piroxicam-loaded microfibers, the presence of small amounts of crystalline drug was observed under polarized light microscopy and in Fourier transform infrared spectra. Drug dissolution performance was evaluated under both sink and non-sink conditions and was found to be significantly enhanced compared to the corresponding crystalline physical mixtures and pure drugs, with evidence of supersaturation behavior noted under non-sink conditions. This study has demonstrated that microfiber-based dispersions may be manufactured by the centrifugal spinning process and may possess characteristics that are favorable for the enhanced dissolution and oral absorption of drugs. © 2016 The Authors

Generation and characterization of standardized forms of trehalose dihydrate and their associated solid-state behavior

Trehalose dihydrate is a nonreducing disaccharide which has generated great interest in the food and pharmaceutical industries. However, it is well recognized that considerable batch to batch variation exists for supposedly identical samples, particularly in terms of the thermal response. In this investigation, two standardized forms of trehalose dihydrate were generated using two distinct crystallization pathways. The two batches were characterized using scanning electron microscopy, X-ray powder diffraction, and FTIR. The thermal responses of the two forms were then studied using modulated temperature differential scanning calorimetry (MTDSC) and thermogravimetric analysis (TGA). In particular, we describe the technique of quasi-isothermal MTDSC as a means of studying the change in equilibrium heat capacity as a function of temperature. Finally, variable temperature FTIR was utilized to assess the change in bonding configuration as a function of temperature. SEM revealed significant differences in the continuity and grain structure of the two batches. The TGA, MTDSC, and quasi-isothermal MTDSC studies all indicated significant differences in the thermal response and water loss profile. This was confirmed using variable temperature FTIR which indicated differences in bond reconfiguration as a function of temperature. We ascribe these differences to variations in the route by which water may leave the structure, possibly associated with grain size. The study has therefore demonstrated that chemically identical dihydrate forms may show significant differences in thermal response. We believe that this may assist in interpreting and hence controlling interbatch variation for this material