Determination of Tranexamic Acid Using Ethyl Chloroformate as Derivatizing Reagent in Pharmaceutical Preparations and Blood by GC

Ethyl chloroformate was used as a derivatizing reagent to develop a simple and sensitive gas chromatographic procedure for the determination of tranexamic acid. Analysis was performed on an HP-5 column (30 m × 0.32 mm i.d.) coupled with mass spectrometric detection. Linear response was obtained from 60 to 500 pg with a limit of detection of 20 pg tranexamic acid injected onto the column. Aminocaproic acid was used as an internal standard. Tranexamic acid was determined in pharmaceutical preparations and blood samples after therapy with the drug. Appoximately 2.0 μg mL^?1 was found in blood samples. Relative standard deviation for analysis was within 0.1–0.4% (n = 3). Recovery of tranexamic acid added to deprotenized serum was 99.6% with an RSD of 1.2–1.6% (n = 3). Pharmaceutical additives and amino acids, if also present, did not affect the determination.     

Intramolecular hydrogen bonding in 3‐imino‐propenylamine: Theoretical investigations

Intramolecular H‐bonds existing for derivatives of 3‐imino‐propenylamine have been studied using the B3LYP/6‐311++G** level of theory. The nature of these interactions, known as resonance‐assisted hydrogen bonds, has been discussed. Vibrational frequencies for α‐derivatives were calculated at the same level of theory. The topological properties of the electron density distributions for N? H···N intramolecular bridges have been analyzed in terms of the Bader theory of atoms in molecules (AIM). Calculation for 3‐imino‐propenylamine derivatives in water solution were also carried out at B3LYP/6‐311++G** level of theory. Finally, the analysis of hydrogen bond in this molecule and their derivatives by quantum theory of natural bond orbital methods fairly support the ab initio results. © 2009 Wiley Periodicals, Inc. Int J Quantum Chem, 2009     

High sensitive determination of trace amount of cobalt by catalytic adsorptive stripping voltammetry

A very sensitive and selective catalytic adsorptive cathodic stripping procedure for trace measurements of cobalt is presented. The method is based on adsorptive accumulation of cobalt-CCA (calcon carboxylic acid) complex onto a hanging mercury drop electrode followed by reduction of the adsorbed species by voltammetric scan using differential pulse modulation. The reduction current is enhanced catalytically by nitrite. The effect of various parameters such as pH, concentration of CCA, concentration of nitrite, accumulation potential and accumulation time on the selectivity and sensitivity were studied. The optimum condition for the analysis of cobalt, include pH 5.2 (Acetate buffer), 2.1 μM clacon carboxylic acid, 0.032 M sodium nitrite and an accumulation potential of 0.05 V (versus Ag/AgCl). Under these optimum conditions and for an accumulation time of 60 s, the measured peak current at −0.480 V is proportional to the concentration of cobalt over the entire concentration range tested 0.003–2.0 ng ml⁻¹ with a detection limit of 1 pg ml⁻¹ for an accumulation time of 60 s and 2.0–10.0 ng ml⁻¹ for an accumulation time of 40 s. The relative standard deviations for ten replicate measurement of 0.5 ng ml⁻¹ of cobalt were 3.1%. The main advantage of this new system is the microtrace Co(II) determination by ASV. The method was applied to determination of cobalt in a water sample and some analytical grade salts with satisfactory results. Published in Elektrokhimiya in Russian, 2009, Vol. 45, No. 2, pp. 221–228. The article is published in the original.     

Multiple Spectroscopic,Docking and Cytotoxic Study of a Synthesized 2,2′ Bipyridin Phenyl Isopentylglycin Pt(II) Nitrate Complex: Human Serum Albumin and Breast Cancer Cell Line of MDA-MB231 as Targets

In the present study, the biological activities of a new synthesized Pt(II)-complex, 2,2′ bipyridinphenyl isopentylglycin Pt(II) nitrate was investigated via its interaction with the most important blood carrier protein of human serum albumin (HSA), using fluorescence and Far-UV circular dichroism (CD) spectroscopic techniques and also molecular docking. Moreover, cytotoxicity activity of the complex was studied against breast cancer cell line of MDA MB231 using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The Pt(II)-complex has a strong ability to quench the intrinsic fluorescence of HSA through a static quenching mechanism. According fluorescence quenching data, the binding parameters of the interaction were calculated and showed that hydrophobic interaction has an important role. The molecular docking results in coherent with fluorescence measurements illustrated that Pt(II) complex can bind to HSA at one position that located in the hydrophobic cavity of groove between drug site I and II. Also, experimental data on driving force in binding site was confirmed whereas theoretical results demonstrated Pt(II) complexinteract to HSA by hydrophobic interaction. Far-UV-CD results showed that Pt(II)-complex induced an increasing in the content of α-helical structure of the protein and stabilized it. Also, MTT assay represented growth inhibitory effect of the complex toward the breast cancer cell line.     

The effect of anodising time on the electrochemical behaviour of the Ti/TiO<Subscript>2</Subscript> NTs/IrO<Subscript>2</Subscript>-RuO<Subscript>2</Subscript>-Ta<Subscript>2</Subscript>O<Subscript>5</Subscript> anode

Nowadays, mixed metal oxide (MMO) anodes are a superior alternative to lead alloys in electrowinning processes. Passivation of titanium substrate is the most common mechanism of deactivation in these anodes. In this research, titanium oxide nanotubes have been utilised as an interlayer between the substrate and a mixed metal oxide coating in order to improve the anode electrochemical behaviour and life via retardation of titanium passivation. Anodising of the substrate was done in 0.5 wt% hydrofluoric acid for 30, 60 and 240 min. The samples were subsequently coated with a coating composed of IrO₂-RuO₂-Ta₂O₅. The microstructure of different samples was observed by scanning with an electron microscope, and the electrochemical behaviour of the samples was studied by accelerated life test, cyclic voltammetry and electrochemical impedance spectroscopy. The studies showed that formation of titanium oxide nanotubes with anodising times of 60 and 240 min increases the life of the anode through the provision of a compact coating. The life of the anode which was anodised for 240 min lasted about 20% longer than the sample which had a substrate without any anodised layer.     

Advantages of using gold hollow nanoshells in cancer photothermal therapy

Lots of studies have been conducted on the optical properties of gold nanoparticles in the first region of near infrared(650 nm–950 nm), however new findings show that the second region of near-infrared(1000 nm–1350 nm) penetrates to the deeper tissues of the human body. Therefore, using the above-mentioned region in photo-thermal therapy(PTT) of cancer will be more appropriate. In this paper, absorption efficiency is calculated for gold spherical and rod-shaped nanoshells by the finite element method(FEM). The results show that the surface plasmon frequency of these nanostructures is highly dependent on the dimension and thickness of shell and it can be adjusted to the second region of near-infrared. Thus, due to their optical tunability and their high absorption efficiency the hollow nanoshells are the most appropriate options for eradicating cancer tissues.     

Improving anti-reflectivity and laser damage threshold of \hbox {SiO}_{2}/\hbox {ZrO}_{2} thin films by laser shock peening at 1064 nm

In this study, anti-reflection (AR) \(\hbox {SiO}_{2}/ \hbox {ZrO}_{2}\) thin films with 3-layers were designed and fabricated by the essential Macleod software and physical vapor deposition, respectively. In order to improve the optical and physical properties of the prepared samples, laser shock peening (LSP) technique was applied. For this purpose, an Argon Fluoride Excimer laser \((\lambda =193 \,\text {nm})\) with 110 and 240 mJ energies and 1 Hz frequency at different pulses was used. The effect of LSP method in improving transmissions and laser damage thresholds of the prepared samples was proved by using UV–Vis–IR spectroscopy in the wavelength range of 400–1200 nm and international standard ISO11254 at 1064 nm. In addition, scanning electron microscopy was used to check the effect of applying LSP.     

An investigation of phenolic compounds from plant sources as trypsin inhibitors

In the search of new trypsin inhibitors caffeic acid (1), cinnamic acid (2), gallic acid (3) and eugenol (4) from Cinnamomum zeylanicum, ferulic acid (5) from Impatiens bicolor, vanillin (6) from Melia azedarach and catechol (7) from Allium cepa were isolated through bioassay guided fractionation of the plant extracts. IC (50) values of the compounds 1, 2 and 5 were found to be 0.35?±?0.02?mM, 0.96?±?0.05?mM and 1.22?±?0.06?mM, respectively. Lineweaver-Burk and Dixon plots and their secondary replots showed that 1 was non-competitive inhibitor of this enzyme with K(i) value 0.102?±?0.006?mM.     

High-efficiency ozone generation via electrochemical oxidation of water using Ti anode coated with Ni–Sb–SnO<Subscript>2</Subscript>

Ozone (O₃) has been generated on Ni–Sb–SnO₂/Ti electrode as anode immersed in acidic media at 25 °C by electrochemical process. The anode was electrochemically characterized by cyclic voltammetry and morphologically characterized by scanning electron microscopy (SEM) and X-ray diffraction. The concentration of dissolved ozone was determined by a UV/Vis spectrophotometer. The type of electrode with different times coating on the titanium mesh and different acid type and various concentrations (C _acid) were used, and the stability of the electrode was investigated under the experimental conditions by SEM images. Results shows that higher efficiency (53.7%) for O₃ generation by electrochemical oxidation of water were obtained in HClO₄ (1 M) and an applied potential of 2.4 V vs. Ag/AgCl in 150 ml volume undivided electrochemical cell.     

Role of Vitamins B-3 and C in the Fashioning of Granules in UASB Reactor Sludge

Whereas a myriad of possible factors have been reported which effect the formation of granules in a upflow anaerobic sludge blanket (UASB) reactor and influence their properties, there is no study on the effect of vitamins on the granulation of UASB reactor sludge. The present study was undertaken to bridge this gap. It was seen that vitamins helped in better granule formation??as reflected by favorable size distribution, sludge volume index, and settling velocity??compared to controls. The vitamin-spiked reactors also achieved >85?% COD removal efficiency in half the number of days the unspiked reactors took. The vitamin supplements were effective at concentrations????1?mg/l. Hence, their use in expediting granule formation as also in developing better-quality granules appears economically viable.