Determination of clonazepam ("Rivotril" or "Ro 5-4023") in plasma by gas chromatography using an internal standard

A method has been developed for gas-chromatographic determination of clonazepam ("Rivotril" or "Ro 5-4023") in plasma, using methyl-clonazepam ("Ro 4082") as an internal standard. Following extraction of the benzodiazepines and hydrolysis, the benzophenones are analyzed by gas-chromatography, using a glass column filled with 3% OV 225 on Gas Chrom Q and a 63Ni electron-capture detector. The technique has good selectivity. The limit of sensitivity is less than 1 ng/ml of plasma. Using this method the plasma kinetics of clonazepam may be studied in man and the correlations between plasma levels and therapeutic activity investigated. It is also available for toxicological analysis, as well as pharmacovigilance purpose. The same internal standard and a similar method can also be used for the determination of flunitrazpem ("Rohypnol" or "Ro 5-4200") and its major metabolite (N-desmethyl-flunitrazepam) in plasma.     

Advanced materials based on new structurally designed poly(naphthylimide‐amide)s

This work reports the synthesis and characterization of novel six‐membered poly(imide‐amide)s based on a naphthalene‐N,N′‐bis(imido‐amine) and various dicarboxylic acids containing flexible units such as ether, hexafluoroisopropylidene and diphenylsilane. A new design is proposed for aromatic poly(imide‐amide)s, in which the imide and amide units are directly connected through a N? N bond. These highly thermostable polymers were successfully synthesized using Yamazaki–Higashi reaction conditions. The poly(imide‐amide)s were processed into thin hydrophobic films having self‐assembled micellar structures. The presence of aggregates in solutions with concentrations below 1% was evidenced and is discussed in relation to the chemical structure. The photoluminescence properties of polymer solutions and films showed their ability to produce white and blue light emission. The lowest unoccupied molecular orbital energy level was calculated using cyclic voltammetry data, showing good electron injection and transport characteristics. The properties of these polymers make them attractive for applications in advanced optoelectronics and related fields. © 2014 Society of Chemical Industry     

Overview of non-destructive evaluation techniques for metal-based additive manufacturing

Three-dimensional printing/digital or additive manufacturing is an area that is taking off with considerable rapidity and magnitude. In the same time, non-destructive evaluation (NDE) is playing an important role in the acceptance of additively manufactured parts, in order to provide the required confidence in the quality of the part and its expected safety and performance while in service. This article represents a summary addressing the subject of applicable NDE techniques to detect manufacturing anomalies and service-induced flaws. The topic is relatively new, attracting much research attention and funding, while in the meantime manufacturing processes are continuously improving. The number of publications covering additive manufacturing is increasing exponentially, and everyday new articles, conferences, and workshops are bringing out new information.     

Analysis of Nonlinear Spectral Eddy-Viscosity Models of Turbulence

Fluid turbulence is commonly modeled by the Navier-Stokes equations with a large Reynolds number. However, direct numerical simulations are not possible in practice, so that turbulence modeling is introduced. We study artificial spectral viscosity models that render the simulation of turbulence tractable. We show that the models are well posed and have solutions that converge, in certain parameter limits, to solutions of the Navier-Stokes equations. We also show, using the mathematical analyses, how effective choices for the parameters appearing in the models can be made. Finally, we consider temporal discretizations of the models and investigate their stability.     

Increasing the adsorption capacity and selectivity of poly(vinyl alcohol) hydrogels by an alternative imprinting technique

In this work, we report an innovative alternative imprinting method for obtaining chemically crosslinked poly(vinyl alcohol) hydrogels with β‐cyclodextrin as template. The materials present high affinity toward the template that imprinted them, revealed by the higher sorption yield of β‐cyclodextrin and higher selectivity factors of the imprinted material, by comparing with the nonimprinted reference. The imprinting kinetic and mechanism has been demonstrated by adsorption studies, binding isotherms and Scatchard analysis and is in good correlation with the information regarding the morphology of the materials, determined by fluorescence microscopy and atomic force microscopy. By using a novel fluorescence spectroscopy method of the starting polymer solution, the optimum amount of imprinting template could be determined. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42024.     

Poly-phenothiazine derivative-modified glassy carbon electrode for NADH electrocatalytic oxidation

Electropolymerization of a new phenothiazine derivative (bis-phenothiazin-3-yl methane; BPhM) on glassy carbon (GC) electrode generates a conducting film of poly-BPhM, in stable contact with the electrode surface. The heterogeneous electron-transfer process corresponding to the modified electrode is characterized by a high rate constant (50.4 s⁻¹, pH 7). The GC/poly-BPhM electrode shows excellent electrocatalytic activity toward NADH oxidation. The rate constant for catalytic NADH oxidation, estimated from rotating disk electrode (RDE) measurements and extrapolated to zero concentration of NADH, was found to be 9.4 × 10⁴ M⁻¹ s⁻¹ (pH 7). The amperometric detection of NADH, at +200 mV vs. SCE, is described by the following electroanalytical parameters: a sensitivity of 1.82 mA M⁻¹, a detection limit of 2 μM and a linear domain up to 0.1 mM NADH.     

Characterization and deposition behavior of silk hydrogels soaked in simulated body fluid

This paper reports the mineralization ability of semi-interpenetrating networks composed of regenerated silk fibroin and polyacrylamide hydrogels soaked in simulated body fluid (SBF1x). Hydrogels were prepared by polymerization of acrylamide and N,N′-methylenebisacrylamide in silk fibroin solution with a redox pair as initiator. The incorporation of the fibroin within the polyacrylamide matrix was proved by FTIR–ATR spectroscopy. Swelling measurements in saline solution were performed to evaluate the behavior of these hydrogels having various compositions. Mineralization assays in SBF1x solution revealed the presence of apatite-like crystals onto the surface of the silk fibroin/polyacrylamide hydrogels. Cytotoxicity test by extract method revealed that these hydrogels with various contents in silk fibroin have not developed cytotoxic effects on human fibroblast cultures which increases the possibility of their use in biomedical applications. Mechanical compressive tests revealed good strengths for silk fibroin/polyacrylamide hydrogels. In this way, organic–inorganic hybrids analogous to bone structure can be produced under biomimetic conditions and could be further used in biomedical applications.     

Morphological, optical and electrical properties of samarium oxide thin films

We present here results on samarium oxide thin films, obtained by pulsed laser deposition and by radio frequency assisted pulsed laser deposition. Three different substrate types were used: silicon, platinum covered silicon and titanium covered silicon. The influence of the deposition parameters (oxygen pressure and laser fluence) on the structure and morphology of the thin films was studied. The substrate-thin film interface zone was investigated; the optical and electrical properties (the losses, dielectric constant and leakage currents) were also determined.     

Differential impedance spectroscopy for monitoring protein immobilization and antibody-antigen reactions

This work describes the theoretical and experimental approaches for monitoring the interfacial biomolecular reaction between immobilized antibody and the antigen binding partner using novel differential impedance spectroscopy. The prerequisite of any biosensor is the immobilization of macromolecules onto the surface of a transducer. It is clear that the function of most macromolecules changes from what is observed in solution once immobilization has occurred. In the worst case, molecules entirely lose their binding activity almost immediately after immobilization. Certain conditions (e.g., denaturation, interfacial effects based on ionic strength, surface charge, dielectric constants, etc.) at interfaces are responsible for alterations of binding activity; it is not clear whether a combination of such processes is understood. However, these processes in combination must be reliably modeled in order to predict the outcome for most macromolecules. This work presents the theoretical and practical means for elucidating the surface reactivity of biomolecular reagents using ion displacement model with antibody-antigen (Ab-Ag) reaction as the test case. The Ab-Ag reaction was directly monitored using a dual-channeled, impedance analyzer capable of 1 measurement/s using covalent immobilization chemistry and polymer-modified electrodes in the absence of a redox probe. The evidence of Ab-Ag binding was revealed through the evolution of differential admittance. The surface loading obtained using the covalent immobilization chemistry was 9.0 x 10(16)/cm2, whereas with polymer-modified electrodes, the surface loading was 9.0 x 10(15)/cm2, representing a 10 times increase in surface reactivity. The proposed approach may be applicable to monitoring other surface interfacial reactions such as DNA-DNA interactions, DNA-protein interactions, and DNA-small molecule interactions.