Comparison and Validation of Drug Loading Parameters of PEGylated Nanoparticles Purified by a Diafiltration Centrifugal Device and Tangential Flow Filtration

This article describes drug loading validation of nanoparticles. Ultracentrifugation was avoided because of problems arising from small-sized particles. Ultrafiltration was adopted in two different modes followed by monitoring of polyvinyl alcohol (PVA), dextran sulfate (DS), and loperamide HCl contents. Diafiltration centrifugation removed all PVA at the fourth cycle and provided significantly (p = .000, .017) higher drug loading values compared with tangential flow filtration (TFF). This was due to residual PVA associated with the nanoparticles. TFF enabled satisfactory dry weight recovery (101.66 ± 4.45%, n = 3) of nanoparticles during extended purification. Indirect drug loading (from the purification curve) was not significantly different (p = .450, .487) to the direct drug loading values. Encapsulation parameters were obtained from the purification curve once quantitative estimation of the all formulation components was established.     

Interactions between shrinkage reducing admixtures (SRA) and cement paste's pore solution

Shrinkage reducing admixtures (SRA) have been developed to combat shrinkage cracking in concrete elements. While SRA has been shown to have significant benefits in reducing the magnitude of drying and autogenous shrinkage, it has been reported that SRA may cause a negative side effect as it reduces the rate of cement hydration and strength development in concrete. To examine the influence of SRA on cement hydration, this study explores the interactions between SRA and cement paste's pore solution. It is described that SRA is mainly composed of amphiphilic (i.e., surfactant) molecules that when added to an aqueous solution, accumulate at the solution-air interface and can significantly reduce the interfacial tension. However, these surfactants can also self-aggregate in the bulk solution (i.e., micellation) and this may limit the surface tension reduction capacity of SRA. In synthetic pore solutions, SRA is observed to form an oil-water-surfactant emulsion that may or may not be stable. Specifically, at concentrations above a critical threshold, the mixture of SRA and pore fluid is unstable and can separate into two distinct phases (an SRA-rich phase and an SRA-dilute phase). Further, chemical analysis of extracted pore solutions shows that addition of SRA to the mixing water depresses the dissolution of alkalis in the pore fluid. This results in a pore fluid with lower alkalinity which causes a reduction in the rate of cement hydration. This may explain why concrete containing SRA shows a delayed setting and a slower strength development.     

Electroanalytical studies on cadmium(II) selective potentiometric sensors based on t-butyl thiacalix[4]arene and thiacalix[4]arene in poly(vinyl chloride)

Cd²⁺-selective sensors have been fabricated from poly(vinyl chloride) (PVC) matrix membranes containing t-butyl thiacalix[4]arene (I) and thiacalix[4]arene (II) as electroactive materials. The addition of sodium tetraphenylborate and the plasticizer 2-nitrophenyl octyl ether has been found to improve the performance of the sensors substantially. The membranes of various compositions of the two thiacalixarenes have been investigated and it was found that the best performance was obtained for the membrane of composition II:PVC:NaTPB:NPOE in the ratio 5:120:3:150. The sensor shows a linear potential response for Cd²⁺ over a wide activity range 3.2 × 10⁻⁶ to 1.0 × 10⁻¹ M with Nernstian compliance (29.5 mV decade⁻¹ of activity) in pH range 4.5-6.5 and a fast response time of ∼8 s. The potentiometric selectivity coefficient values determined by matched potential method indicate excellent selectivity for Cd²⁺ ions over mono-, di- and trivalent interfering cations. The sensor exhibits adequate shelf life (∼3 months) with good reproducibility (S.D. ±0.2 mV) and can also be used in partially non-aqueous media having up to 20% (v/v) methanol, ethanol or acetone content with no significant change in the value of slope or working activity range. The sensor has been used in the potentiometric titration of Cd²⁺ with EDTA. The sensor could be successfully used for the quantification of cadmium in river water samples.     

The kinetics of CNT transfer between immiscible blend phases during melt mixing

The complete transfer of multiwalled carbon nanotubes (MWCNTs) from a poly(styrene acrylonitrile) (SAN) precompound into an initially unfilled polycarbonate (PC) phase during 5 min of discontinuous melt mixing in a microcompounder has been observed recently. However, the typical time scale of the occurring transfer is presently still unknown. Morphological investigations within our study revealed that similar results can be obtained when the SAN-MWCNT-precompound is melt blended with neat PC by continuous twin-screw extrusion. Additionally, the kinetics of the CNT transfer was also investigated in a kneading chamber. We found that the CNT transfer rate turned out to be strongly coupled to the development of the interfacial area of the blend. Furthermore, we evaluated the interplay and significance of the possible and presently only insufficiently understood transfer mechanisms. We proposed for the first time a correlation between major processing and blend parameters and the probability of carbon nanotube transfer due to the development of a nanoscaled wetting angle.     

Efficient Implicit Finite-Element Hydrodynamic Model for Dam and Levee Breach

This technical paper presents the development and application of a pseudo-transient continuation (PTC)– inspired flow model for the simulation of dam and levee failure. The unstructured, implicit, Petrov-Galerkin finite-element model relies on computed residuals to automatically adjust the time-step size. The implicit time integration, together with the automatic time-step size selection through PTC, makes the model computationally efficient. The model is verified and applied to several analytic and real-world test cases that exercise model behavior and accuracy for several critical, transcritical, and subcritical flows. The result is an efficient and accurate prediction of both the speed and depth of shock waves as the dam-break flow passes over initially dry and wet land.     

Influence of multiple gas inlet jets on fluidized bed hydrodynamics using Particle Image Velocimetry and Digital Image Analysis

A rectangular fluidized bed setup was developed to study the evolution of inlet gas jets located at the distributor. Experiments were conducted with varying distributor types and bed media to understand the motion of particles and jets in the grid-zone region of a fluidized bed. Particle Image Velocimetry and Digital Image Analysis were used to quantify the parameters that characterize these jets. A grid-zone phenomenological model was developed to compare these parameters with those available in the literature. It was determined from this study that jet penetration length behavior is consistently different for fluidization velocities below and above the minimum fluidization. For velocities above minimum fluidization, jet lengths were found to increase more rapidly with increase in orifice velocity than for operating conditions below minimum fluidization.     

Influences of polymer matrix melt viscosity and molecular weight on MWCNT agglomerate dispersion

In order to study the influence of melt viscosity and molecular weight on nanotube dispersion and electrical volume resistivity, three different polycarbonates (PCs) varying in molecular weight were melt compounded with 1 wt% multiwalled carbon nanotubes (MWCNTs, Baytubes^® 150 HP) using a small-scale compounder. The experiments were performed at constant melt temperature but at varying mixing speeds, thereby applying different magnitudes of shear stress. Light transmission microscopy was used to access the state of agglomerate dispersion, and electrical resistivities of the composites were measured on pressed plates. The results indicate that with increasing matrix viscosity the agglomerate dispersion gets better when using constant mixing conditions but worse considering comparable shear stress values. To study the effect of molecular weight, in a second set of experiments melt temperatures were adjusted so that all PCs had similar viscosity and mixing was performed at constant mixing speed. As investigated on two viscosity levels, the composites based on the low molecular weight matrix showed smaller sized un-dispersed primary agglomerates as compared to composites with higher molecular weight matrices, highlighting the role of matrix infiltration into primary nanotube agglomerates as the first step of dispersion. The resistivity values of composites prepared using low viscosity matrices were lower than those of composites from high viscosity matrix.     

Formulation development and optimization of alpha ketoglutarate nanoparticles for cyanide poisoning

The purpose of this research work was to formulate and evaluate alpha ketoglutarate nanoparticles as dry powder inhaler for treatment of cyanide poisoning. Non-polymeric particles were prepared by nano-precipitation technique using various stabilizers. Selection of co-solvent and stabilizer was a key to produce stabilized particles. A combination of lutrol F68 and PVA as a crystal growth inhibitor seems to be best in achieving minimum particle size of 110.2 nm. On the basis of preliminary trials a Box-Behnken statistical design was employed to study the effect of independent variables, drug concentration (X₁), stirring speed (X₂), stirring time (X₃), PVA concentration (X₄), poloxomer concentration (X₅) and volume of co-solvent (X₆) on average particle size. Particle size varied from 110 to 875 nm depending upon the significant terms. Optimized formulation was predicted at drug concentration (50 μg/ml), stirring speed (640 rpm), stirring time (1 min), PVA concentration (1%), poloxomer concentration (1.69%) and volume of co-solvent (30 ml) with 104.6% experimental validity. The nanosized particles were further characterized by X-ray diffraction (XRD), Differential Scanning Calorimetry (DSC), Nuclear Magnetic Resonance (NMR) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. The results of particle characterization indicate that there was no physical disparity when compared with the commercial α-KG sample.