A Validated RP–LC Method for Simultaneous Determination of Losartan Potassium and Amlodipine Besilate in Pharmaceutical Preparations

A simple RP–LC method for simultaneous quantification of losartan and amlodipine and separation of their degradation products has been developed. For this purpose we tested appropriated mobile phase pH range, flow rate, temperature and different columns. The method was validated with an ODS column. A gradient of acetonitrile and phosphate pH 3.0 buffer was utilized as mobile phase. The linearity was determined at 50–150% level. Individual recoveries at 70–130% level ranged from 98.8 to 100.5% for losartan and 96.4–101.2% for amlodipine. The robustness was also evaluated. Although losartan has much higher quantities than amlodipine in commercial tablets, this method allowed simultaneous quantification for both drugs.     

An HPLC method for the determination of adenosine diphosphate: An important marker of hexokinase activity in metabolic diseases

Hexokinases play a critical role in the cellular uptake and utilization of glucose. As such, they are of fundamental importance to all cells. By catalyzing glucose to produce glucose‐6‐phosphate, hexokinases control the first irreversible step of glucose metabolism and initiate all major pathways of glucose consumption. Our objective was to develop and validate highly sensitive and selective high‐performance liquid chromatography with photodiode array detector (HPLC‐PDA) assays allowing the determination of adenosine diphosphate, which was used for the determination of hexokinase activity. Samples were analyzed by HPLC‐PDA using a C₁₈ analytical column (250 × 4.6 mm) for chromatographic separation. Optimal detection was achieved based on isocratic elution with a mobile phase consisting of a mixture of sodium phosphate monobasic buffer and methanol. This method met all of the requirements of specificity, sensitivity, linearity, precision, accuracy and stability generally accepted in bioanalytical chemistry and was successfully applied to a study of hexokinase activity in an alloxan‐induced diabetic rat model. Determination of hexokinase activity will permit characterization of cellular metabolic state in many diseases, such as cancer and diabetes.     

SERS and Raman imaging as a new tool to monitor dyeing on textile fibres

Textile fibres containing Ag nanoparticles have been widely explored for a number of antimicrobial fabrics. Moreover, it is well‐known that textile dyeing is a critical stage in the manufacture thereof. This research shows that surface enhanced Raman scattering (SERS) and Raman imaging can be used with advantage in the monitoring of this process. Using Ag containing linen fibres stained with methylene blue (MB), it was possible to map the local distribution of the MB dye in the fibres by Raman imaging. MB was selected as the SERS molecular probe and as a model dye. Composites of linen fibres and Ag nanoparticles were prepared by distinct methods and used as SERS substrates in order to evaluate the effect of the preparative method on the Raman images. Our results demonstrate that by using Raman imaging associated to the presence of Ag nanoparticles, it is possible to distinguish the local distribution of the dye on the textile surface. This investigation allows to foreseeing the use of this technique in terms of quality control of Ag containing fabrics, which is a market in great expansion. Copyright © 2016 John Wiley & Sons, Ltd.     

Kinetic Analysis of the Decomposition of Chelates of Di-alkyldithiocarbamate of Cd(II)

The thermal decomposition kinetics of the solid complexes Cd(S₂ CNR₂ )₂ , where R =C₂ H₅ , n -C₃ H₇ , n -C₄ H₉ or iso -C₄ H₉ , was studied by using isothermal and non-isothermal thermogravimetry. The superimposed TG/DTG/DSC curves revealed that thermal decomposition reactions occur in the liquid phase. The kinetic model that best fitted the experimental isothermal TG data was the one-dimensional phase-boundary reaction-controlled process R₁ . The thermal analysis data suggested the thermal stability sequence Cd(S₂ CNBuⁿ ₂ )₂ >Cd(S₂ CNPrⁿ ₂ )₂ >Cd(S₂ CNBuⁱ ₂ )₂ >Cd(S₂ CNEt₂ )₂ , which accords with the sequence of stability of the apparent activation energies. This revised version was published online in July 2006 with corrections to the Cover Date.     

Antioxidant defenses and DNA damage induced by UV-A and UV-B radiation in the crab Chasmagnathus granulata (Decapoda, Brachyura)

The photoprotector role of pigment dispersion in the melanophores of the crab, Chasmagnathus granulata, against DNA and oxidative damages caused by UV-A and UV-B was investigated. Intact and eyestalkless crabs were used. In eyestalkless crabs, the dorsal epidermis of the cephalothorax (dispersed melanophores) and the epidermis of pereiopods (aggregated melanophores) were analyzed. Intact crabs showed only dispersed melanophores in the two epidermis. Antioxidant enzymes activity and lipoperoxidation content were analyzed after UV-A (2.5 J/cm2) or UV-B (8.6 J/cm2) irradiation. DNA damage was analyzed by single cell electrophoresis (comet) assay, after exposure to UV-B (8.6 J/cm2). UV-A radiation increased the glutatione-S-transferase activity in the pereiopods epidermis of eyestalkless crabs (P<0.05). UV-B radiation induced DNA damage in the dorsal epidermis of eyestalkless crabs (P<0.05). In pereiopod epidermis of eyestalkless crabs, there was no significant difference between control and UV-B-exposed crabs. In the pereiopods epidermis of eyestalkless, the control group showed higher scores of DNA damage and approximately 50% of cellular viability. Because in eyestalkless and irradiated crabs the cellular viability was approximately 5%, it was not possible to observe nuclei for determination of DNA damage. The findings show that melanophores can play a role in the defense against harmful effects of a momentary exposure to UV radiation.     

Preparation of nanocomposites by reversible addition‐fragmentation chain transfer polymerization from the surface of quantum dots in miniemulsion

Herein, we report the synthesis of quantum dots (QDs)/polymer nanocomposites by reversible addition‐fragmentation chain transfer (RAFT) polymerization in miniemulsions using a grafting from approach. First, the surfaces of CdS and CdSe QDs were functionalized using a chain transfer agent, a trisalkylphosphine oxide incorporating 4‐cyano‐4‐(thiobenzoylsulfanyl)pentanoic acid moieties. Using a free radical initiator (AIBN) to activate the RAFT process, a polystyrene (PS) block was grafted from the surface of the QDs. Quantum confinement effects were identified for the nanocomposite obtained, so attesting to the integrity of the QDs after the polymerization. Free PS chains were also present in the final nanocomposite, indicating that the RAFT polymerization from the surface of the QDs was accompanied by conventional free radical polymerization. After isolating the nanocomposite particles, a second poly(n‐butyl acrylate) block was tentatively grown from the initial PS block. The first results indicated a successful polymerization of the second polymer and show the potential of the current strategy to prepare block copolymers from the surface of the RAFT‐modified QDs. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 5367–5377, 2009     

Hardness anomalies on Cr 1−x Fe x (0.05<x<0.323) alloys: Mössbauer effect study

The hardness of Cr_1-xFe_x α solid solutions presents an anomalous behaviour in the range 0.10<xFe<0.30, that has been explained either by magnetic or electronic effects. In order to verify wether the anomalies were intrinsic to that phase or were induced by impurities, measurements of microhardness and isomer shift of samples of high purity Cr_1-xFe_x α solid solutions (0.05<xFe<0.323) were carried out. We found that the hardness presents a maximum and a minimum for xFe-0.19 and xFe-0.17, respectively, which are inferior to the amplitudes of the anomalies found by previous authors using lower purity alloys. Within the limit of experimental error, the isomer shift at room temperature varies linearly with the composition. These results suggest that impurities play a major role in determining the magnitude of the hardness anomalies and that electron transfer varies smoothly in the concentration range studied.