Hollow Multilayer Microcapsules for pH‐/Thermally Responsive Drug Delivery using Aliphatic Poly(urethane‐amine) as Smart Component

Hollow multilayer microcapsules made of aliphatic poly(urethane‐amine) (PUA) and sodium poly(styrene sulfonate) (PSS), templated on PSS‐doped CaCO₃ particles, are prepared for pH‐/thermally responsive drug delivery. The electrostatic interaction and hydrogen bonding under weak‐acid conditions between aliphatic PUA and PSS contribute to the formation of multilayer microcapsules. Scanning electron microscopy (SEM) results demonstrate an obvious variation of the hollow multilayer microcapsules in response to changes in temperature and pH value. Drug‐release behaviors using DOX as a model drug demonstrate that the drug release increases on decreasing the pH value because of the interaction weakness between aliphatic PUA and PSS in acidic conditions. Moreover, the drug release is higher at 55 °C than that at 37 °C for the sake of the shrinkage of aliphatic PUA above its lower critical solution temperature (LCST).

     

Estimation of the breakthrough volume of selected steroids for C‐18 solid‐phase extraction sorbent using retention data from micro‐thin layer chromatography

SPE method is a very popular technique, and is commonly used for the prepurification, concentration, and isolation of different organic compounds from variable matrices. In this work, the optimization of SPE process was carried out. The breakthrough volume of solid sorbents based on octadecylsilane was determined and three methods were compared: (1) calculation one – the breakthrough volume was calculated using retention factor k determined with micro‐TLC method, frontal analysis – (2) breakthrough volume was determined as volume of whole elution peak, and (3) breakthrough volume was determined as the center of peak gravity. For calculation method, the k values of key estrogens and progestogens were derived from the micro‐TLC experiment reported previously. By combining these three methods, we can point the start of elution, the maximum concentration of analyte in eluate, and the whole eluent volume, which is necessary to achieve an appropriate selectivity and high extraction recovery. Proposed calculation method allows to estimate the beginning of the steroid peak, when the analyte appears in the eluate flowing from the sorbent. Such observation advances the SPE optimization protocol that was described before and was based on the correlation between raw k_SPE and k_micro‐TLC data.     

Annealing of silver nanolayers sputtered on polytetrafluoroethylene

Silver nanolayers sputtered on polytetrafluoroethylene and their changes induced by post‐deposition annealing at 100–300 °C are studied. Changes in surface morphology and roughness are examined by atomic force microscopy and by measurement of electrical sheet resistance by two‐point technique. Chemical composition was determined by X‐ray photoelectron spectroscopy (XPS) and electrokinetic analysis in dependence on the gold layer thickness. The annealing at 300 °C leads to significant rearrangement of the silver layer, and the transition threshold increases to 35 nm. The presence of oxidized structures on silver‐coated samples is observed in XPS spectra and by electrokinetic analysis, too. Annealing of pristine and silver‐coated poly(tetrafluoroethylene) at 300 °C results in significant change of the sample surface morphology and chemistry. There is observed formation of isolated silver islands on the surface, which could be connected with silver melting. Later, the silver agglomeration takes place. Copyright © 2013 John Wiley & Sons, Ltd.     

Effects of Ethanol on the Stability of Pigment Colloidal Dispersion

The effects of ethanol on the thickness and ionization of adsorbed polymer layer on pigment were investigated. The results showed that the thickness of adsorbed polymer layer decreased with the increase of the ethanol concentration, and then the pigment particles aggregated when the concentration of ethanol is higher than 40%. The zeta potentials became more negative with the increasing of the ethanol concentration, and then changed reversely when the ethanol concentration was higher than 16%. The thickness and structure of adsorbed polymer layer on the particle determined the stability of pigment dispersion.     

Effect of Discrete Macroion Charge Distributions on Electric Double Layer of a Spherical Macroion

The effect of replacing the conventional uniform macroion surface charge density with discrete macroion charge distributions on the structure of electric double layer (EDL) of a spherical macroion has been investigated by Monte Carlo (MC) simulations. Two discrete models have been investigated in addition to the central macroion charge: point charges localized on the macroion surface and finite-sized charges protruding into the solution. Both models have been studied with fixed and mobile macroion charges. The radial functions of local densities and electrostatic potential in EDL, are calculated and compared to the results obtained for the central macroion charge distribution. It is concluded that the model of charge distribution significantly affects the EDL structure close to the macroion, while the effect is much weaker at larger distances. With point charges localized on the macroion surface, counterions become stronger accumulated to the macroion, as a result the absolute values of surface potential ?₀ and zeta ξ potential are decreased. With protruding charges, the excluded volume effect dominates over the increased correlation ability; hence the counterions are less accumulated near the macroions and the absolute values of ?₀ and ξ potentials are increased.     

Ethylene Glycol as New Mobile Phase for Resolution of Two-Component Mixture of Cationic Surfactants on Alumina Surface

Aqueous ethylene glycol (ethane 1,2 diol) as a green mobile phase has been used for thin layer chromatographic (TLC) studies of cationic surfactants on alumina layers. Nineteen solvent systems were used to examine the mobility of the surfactants and to discover the best TLC system for the selective separation of dodecyl trimethylammonium bromide (DTAB) from multi-component mixture of other surfactants. Among the TLC systems studied, M₃ (ethylene glycol: water, 8:2) was best for achieving the selective separation of DTAB from multi-component mixture of other surfactants because in this mobile phase mobility of all surfactants except DTAB were insignificant. Effect of organic additives in aqueous ethylene glycol mobile phase on the mobility of surfactants was examined. The results obtained on laboratory made alumina TLC plates and commercially available precoated alumina HPTLC plates were compared. The lower limits of detection of DTAB, CPC, CTAB, HDTAC, and TTAB were 0.02, 0.05, 0.04, 0.06, or 0.08 µg per zone respectively. The resolution of mixture of cationic surfactants was also examined in the presence metal cations as an impurity in the analyzed sample.     

Self-constructed stable liquid crystal alignment in a monomer-liquid crystal mixture system

Here, we demonstrate excellent liquid crystal (LC) vertical alignment without using an alignment layer printing process by introducing octadecyltrichlorosilane (OTS) into the LC mixture. Further, we investigated the alignment mechanism by analysing the surfaces of the substrates. The optimum concentration of OTS was found to be about 0.03 wt%, which is 1/100 of that in the previously reported polyhedral oligomeric silsesquioxane (POSS)–LC system. Moreover, the OTS–LC system exhibited a more stable LC alignment compared with the POSS–LC system. These differences may arise from the different strengths of surface–dopant interactions; that is, the covalent bond in the OTS–LC system and the van der Waals interactions in the POSS–LC system. We also demonstrated that the method can be used in a capillary tube, which may serve as a new method facilitating the application of LCs with curved surfaces.     

Investigation on ion movement in the fringe-field switching mode depending on resistivity of alignment layer and dielectric anisotropic sign of liquid crystal

Adsorption and desorption of ions at interface between liquid crystal and alignment layer in liquid crystal displays play a crucial role in residual direct current voltage associated with image sticking. In this article, the dependency of such adsorption and desorption of ions on resistivity of alignment layer and sign of liquid crystal dielectric anisotropy in the fringe-field liquid crystal cell has been investigated. Our studies show that the time constant of ions during adsorption and desorption depends upon resistivity and dielectric constant of liquid crystal and alignment layer, and most strongly influenced by the resistivity of alignment layer such that the one with lower resistivity in two orders shows much faster adsorption and desorption at the interface than that of the one with higher resistivity.     

X-ray diffraction and dielectric spectroscopy studies on a partially fluorinated ferroelectric liquid crystal from the family of terphenyl esters

The fluorinated compound, (S)-4′′-(6-perfluoropentanoyoxyhexyl-1-oxy)-2′,3′-difluoro-4-(1-methylheptyloxycarbonyl)-[1,1′:4′,1′′]-terphenyl, which exhibits antiferroelectric SmC_A*, ferroelectric SmC* and paraelectric SmA* phases, has been investigated by polarising optical microscopy, differential scanning calorimetry, X-ray diffraction and frequency-dependent dielectric spectroscopy methods. X-ray studies have revealed that the layer thickness remains almost constant in the SmA* phase but within the SmC* and SmC_A* phases it decreases with decreasing temperature, a step jump being observed only at the SmA*–SmC* transition. The tilt angle in the SmC_A* phase decreases from 22.2° to 19.5°, and in the SmC* phase it decreases from 18.8° to 5.5°. Spontaneous polarisation is found to be quite high and varies between 74.1 and 118.7 nC cm^?2. The variation in ε′ and ε′′ with temperature shows a discontinuous change at the transition temperatures. Goldstone mode relaxation is only observed in the ferroelectric and antiferroelectric phases and is found to be of the Cole–Cole type. The soft mode is observed on application of a bias field near the SmC*–SmA* transition. Neither the soft mode nor the anti-phase azimuthal angle fluctuation mode is observed in SmC_A*. Rotational viscosity decreases quite rapidly with temperature but in a different manner in the ferroelectric and antiferroelectric phases. Activation energy for this process is found to be 48.14 kJ mol^?1 in the SmC* phase.     

Determination of zinc in marine/lacustrine sediments by graphite furnace atomic absorption spectrometry using Pd/Mg chemical modifier and slurry sampling

Effectiveness of Pd/Mg chemical modifier for the accurate direct determination of zinc in marine/lacustrine sediments by graphite furnace atomic absorption spectrometry (GF-AAS) using slurry samples was evaluated. A calibration curve prepared by aqueous zinc standard solution with addition of Pd/Mg chemical modifier is used to determine the zinc concentration in the sediment. The accuracy of the proposed method was confirmed using Certified Reference Materials, NMIJ CRM 7303-a (lacustrine sediment) from National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology, Japan, and MESS-3 (marine sediment) and PACS-2 (marine sediment) from National Research Council, Canada. The analytical results obtained by employing Pd/Mg modifier are in good agreement with the certified values of all the reference sediment materials. Although for NRC MESS-3 an accurate determination of zinc is achieved even without the chemical modifier, the use of Pd/Mg chemical modifier is recommended as it leads to establishment of a reliable and accurate direct analytical method. One quantitative analysis takes less than 15 minutes after we obtain dried sediment samples, which is several tens of times faster than conventional analytical methods using acid digested sample solutions. The detection limits are 0.13?µg?g^?1 (213.9?nm) and 16?µg?g^?1 (307.6?nm), respectively, in sediment samples, when 40?mg of dried powdered samples are suspended in 20?mL of 0.1?mol?L^?1 nitric acid and a 10?µl portion of the slurry sample is measured. The precision of the proposed method is 8–15% (RSD).