Validated Stability-Indicating Method for Alendronate Sodium Employing Zwitterionic Hydrophilic Interaction Chromatography Coupled with Charged Aerosol Detection

Alendronate sodium is widely used in the treatment of osteoporosis and Paget’s disease. The HPLC method development for alendronate sodium, in particular, is challenging owing to the absence of chromophoric group and its high polarity. In the present study, a short and simple isocratic method was developed involving hydrophilic interaction liquid chromatography, coupled with a charged aerosol detector. The developed method was validated according to the ICH Q2(R1) guideline and was successfully applied for the analysis of a marketed formulation containing the drug.

     

Activation of peroxyl and molecular oxygen using bis -benzimidazole diamide copper (II) compounds

New tetradentatebis-benzimidazole ligands have been synthesized and utilized to prepare copper (II) complexes. Some of these copper (II) complexes have been characterized structurally. The copper (II) in these complexes is found to possess varying geometries. A distorted octahedral geometry is found with a highly unsymmetrical bidentate nitrate group. An unusual polymeric one-dimensional structure is observed where copper (II) is in a distorted square pyramidal geometry with a monodentate nitrate ion, having long Cu-O bond, while a distorted triagonal bipyramidal geometry is found with two carbonyl O atoms and a Cl atom in the equatorial plane, and two benzimidazole imine N atoms occupy the axial position. These compounds are found to activate the cumylperoxyl group, and this has been utilized in the facile oxidation of aromatic alcohols to aldehydes, where they act as catalysts with large turnovers. The yields of the respective products vary from 32 to 65%. The role of molecular oxygen has been studied and an attempt has been made to identify the “active copper species”. Activation of molecular oxygen has also been observed and has been used for oxidative dealkylation of a hindered phenol, producing di-butyl quinones with yields of 20–25% and 10–12 fold catalytic turnover. Dihydroxybenzenes and substituted catechols are also readily oxidized to the corresponding quinones, in oxygen-saturated solvents. Yields of 84% have been observed with 34-fold catalyst turnover, with di-t-butylcatechol. The activity of these copper (II) —bis-benzmidazolediamide compounds is reminiscent of the functioning of copper centres in galactose oxidase, tyrosinase and catechol oxidase.     

The influence of Na<Superscript>+</Superscript> on the anilinepropylsilica xerogel synthesis by using the fluoride nucleophilic catalyst

Anilinepropylsilica xerogel was obtained by using an appropriate organosilane and tetraethyl orthosilicate as precursor reagents. The gelation was carried out using HF and NaF as catalysts. The presence of Na⁺ (when NaF was used) resulted in a decrease in the final organic content of the materials. This effect was interpreted as an inhibition of the organosilane polycondensation possibly due to the Na⁺ interaction with the SiO^- groups of the hydrolyzed organosilane. The presence of Na⁺ also results in morphological changes in the xerogels.     

Fundamental Limitations of Continuous-Time Delta–Sigma Modulators Due to Clock Jitter

We examine noise due to clock jitter in single-loop low-pass continuous-time delta-sigma (Delta Sigma) modulators (CT-DSMs) employing nonreturn to zero (NRZ) feedback digital-to-analog converters (DACs). Using the discrete-time version of the Bode sensitivity integral, we derive a lower bound on jitter noise and its relationship to the noise transfer function (NTF) of the modulator. We show that NTFs with optimized zeros result in lower jitter noise than those with all zeros at the origin. We give intuition to a recent observation (arrived through numerical optimization) that NTFs with peaking in their passbands have lower jitter noise than maximally flat NTFs. We propose a design procedure that minimizes the sum of the quantization and jitter noise. The arguments regarding Delta Sigma analog-to-digital converters are extended to Delta Sigma DACs and measurement results are presented.     

Supporting real-time and multimedia applications on the Mercuritestbed

This paper describes the distributed system, network and software architecture, the application development environment, the performance, and the early lessons learned on the ATM LAN testbed Mercuri established at the Honeywell Technology Center, to develop distributed multimedia technologies for real-time control applications. We have developed a client-server-based software architecture on Sun Sparcstation-2s connected by a Fore Systems' ASX-100 ATM switch, with video processing handled by Parallax's X Video cards. The architecture enables network-transparent applications and provides simple primitives for multimedia capture, display, transmission, storage, and retrieval. A real-time multimedia-in-the-loop control application was developed as the vehicle for testing the capabilities and performance of the network. Our test measurements focus on the end-user-level performance metrics such as message throughput and round-trip delay as well as video-frame jitter under no-load and load conditions. Our results show that the maximum burst throughput that can be supported at the user level is 48 Mb/s using AAL 5, while round-trip delays for 4-kbyte messages are about 3 ms. Our experience reveals a number of performance bottlenecks and open issues in using commercial ATM switches for practical applications. Our conclusions are outlined     

Influence of impact-ionization-induced base current reversal onbipolar transistor parameters

In this paper we describe a set of measurements representing a complete characterization of impact-ionization effects in bipolar transistors. We demonstrate that impact-ionization significantly influences the dependence of base resistance on current and voltages applied to the device. A dc method for the simultaneous extraction of all parasitic resistances in bipolar transistors is presented. The method can separate the influence of current-crowding on the base resistance from that of base width and conductivity modulation; the collector parasitic resistance is measured in the active region. Starting from the parameters extracted by means of these techniques, a complete and accurate circuit-model of impact-ionization effects can be defined     

g-Factor of the first 2+ state in theN=82 nucleus138Ba

The 2 ₁ ⁺ level of¹³⁸Ba has been Coulomb excited with a 105 MeV³²S beam. The precession of the gamma ray angular distribution induced by the transient magnetic field when traversing a 2.14 mg/cm² iron foil, has been measured to be 15.6(1.7) mr. A value of g(¹³⁸Ba 2 ₁ ⁺ )=0.72(11) was obtained assuming for the transient field strength the Chalk River calibration. The field parametrization has been checked using the first 2⁺ state in¹⁵⁰Sm as probe. Theg value obtained is sensibly lower than predicted by large scale shell model calculations in a proton subspace. Theg-factor of the first 2⁺ state in¹⁴⁸Sm has been remeasured yieldingg(¹⁴⁸Sm 2 ₁ ⁺ )=0.246(22).     

Chemical, structural, and thermal properties of Zn(II)-Cr(III) layered double hydroxides intercalated with sulfated and sulfonated surfactants

Zn(II)-Cr(III)-LDHs (layered double hydroxides) containing sulfated or sulfonated surfactants as the interlamellar anion were synthesized by the coprecipitation method. The syntheses were conducted under various different experimental conditions, such as the Zn : Cr ratio, pH, and aging time. In each of the prepared materials, unlike previously reported data, the interlayer anion arrangement did not change, being consistent with a perpendicular monolayer. The thermal decomposition process of the prepared materials was studied by a set of analysis methods, such as TG/DTA, TG/MS, PXRD, and FT-IR. From the results obtained it was possible to conclude that, in an air atmosphere, the anions decomposed by a partial combustion, leading to the formation of sulfide. The results also showed that sulfonated surfactants containing LDHs are much more stable than those containing sulfated surfactants. A mechanism was proposed for the thermal decomposition of such LDHs based on the experimental results.