Design and Synthesis of New Chacones Substituted with Azide/Triazole Groups and Analysis of Their Cytotoxicity Towards HeLa Cells

A series of new chalcones substituted with azide/triazole groups were designed and synthesized, and their cytotoxic activity was evaluated in vitro against the HeLa cell line. O-Alkylation, Claisen-Schmidt condensation and Cu(I)-catalyzed cycloaddition of azides with terminal alkynes were applied in key steps. Fifteen compounds were tested against HeLa cells. Compound 8c was the most active molecule, with an IC₅₀ value of 13.03 μM, similar to the value of cisplatin (7.37 μM).     

Sewage sludge coke estimation using thermal analysis

The imposition of more stringent legislation by CETESB in the State of São Paulo (Brazil) governing the disposal and utilization of sewage sludge, coupled with the growth in its generation has prompted a drive for alternative uses of sewage sludge. One option that is especially promising, due to its potential to valorize sludge, is its conversion into carbonaceous adsorbents or coke for industrial effluents treatment. Thus, a methodology is presented to estimate the coke produced from the sludge of a sewage treatment station using thermal analysis. The used sewage sludge, which comes from aerobic treatment, was collected in the wastewater treatment station of Barueri, one of the largest of the São Paulo metropolitan area. The sludge samples were collected, dried, ground, and milled until they passed an ABNT 200 sieve. The inert ambient used during its thermal treatment produces inorganic matter and coke as residual materials. Coke formation occurs in the 200–500 °C range and, between 500 and 900 °C, its thermal decomposition occurs. The highest formation of coke occurs at 500 °C.     

Terpenoids from Croton regelianus

Two new terpenoids, the bisnorditerpene rel‐(5β,8α,10α)‐8‐hydroxy‐13‐methylpodocarpa‐9(11),13‐diene‐3,12‐dione ( 1 ) and the guaiane sesquiterpene rel‐(1R,4S,6R,7S,8aR)‐decahydro‐1‐(hydroxymethyl)‐4,9,9‐trimethyl‐4,7‐(epoxymethano)azulen‐6‐ol ( 2 ), together with seven known compounds, were isolated from Croton regelianus var. matosii. The structures of the isolated compounds were determined by HR‐ESI‐TOF and a combination of 1D‐ and 2D‐NMR experiments.     

Enzymatic resolution of racemic sulcatol by lipase from Candida Antarctica in a large scale

Large scale enzymatic resolution of racemic sulcatol 2 has been useful for stereoselective biocatalysis. This reaction was fast and selective, using vinyl acetate as donor of acyl group and lipase from Candida antarctica (CALB) as catalyst. The large scale reaction (5.0 g, 39 mmol) afforded high optical purities for S-(+)-sulcatol 2 and R-(+)-sulcatyl acetate 3, i.e., ee > 99 per cent and good yields (45 per cent) within a short time (40 min). Thermodynamic parameters for the chemoesterification of sulcatol 2 by vinyl acetate were evaluated. The enthalpy and Gibbs free energy values of this reaction were negative, indicating that this process is exothermic and spontaneous which is in agreement with the reaction obtained enzymatically.     

Efficient global optimization algorithm assisted by multiple surrogate techniques

Surrogate-based optimization proceeds in cycles. Each cycle consists of analyzing a number of designs, fitting a surrogate, performing optimization based on the surrogate, and finally analyzing a candidate solution. Algorithms that use the surrogate uncertainty estimator to guide the selection of the next sampling candidate are readily available, e.g., the efficient global optimization (EGO) algorithm. However, adding one single point at a time may not be efficient when the main concern is wall-clock time (rather than number of simulations) and simulations can run in parallel. Also, the need for uncertainty estimates limits EGO-like strategies to surrogates normally implemented with such estimates (e.g., kriging and polynomial response surface). We propose the multiple surrogate efficient global optimization (MSEGO) algorithm, which adds several points per optimization cycle with the help of multiple surrogates. We import uncertainty estimates from one surrogate to another to allow use of surrogates that do not provide them. The approach is tested on three analytic examples for nine basic surrogates including kriging, radial basis neural networks, linear Shepard, and six different instances of support vector regression. We found that MSEGO works well even with imported uncertainty estimates, delivering better results in a fraction of the optimization cycles needed by EGO.     

A new approach to ion exchange chromatography with conductivity detection for adulterants investigation in dietary supplements

The extent of adulteration of dietary supplements has significantly increased in recent years. This situation worries health authorities and requires auxiliary analytical tools for the investigation of illegal substances purposely added. Ion exchange chromatography with conductivity detection is a consolidated analytical technique for the determination of inorganic compounds in various matrices. This technique has been applied to the pharmaceutical characterization of mainly impurities and degradation products. This work presents a new approach to ion exchange chromatography as a screening method to investigate the presence of amfepramone, femproporex, sibutramine, bisacodyl and amiloride in dietary supplements advertised for weight loss. The method was optimized and validated using a Metrosep C4 100/4.0 cation exchange column. The mobile phase consisted of 1.8 mm HNO₃ containing 2% acetonitrile (v/v), with a flow rate of 0.9 ml min^?1, and nonsuppressed conductivity detection was applied. The limits of detection and quantification varied from 1.01 to 3.62 mg L^?1 and from 1.48 to 8.72 mg L^?1, respectively. The proposed method was successful applied to 78 solid dietary supplement samples, in two of which adulterations were found. Moreover, ion exchange chromatography with conductivity detection could be easily used for quality control without prior complex sample pre‐treatment.     

Dynamical analysis of turbulence in fusion plasmas and nonlinear waves

Turbulence is one of the key problems of classical physics, and it has been the object of intense research in the last decades in a large spectrum of problems involving fluids, plasmas, and waves. In order to review some advances in theoretical and experimental investigations on turbulence a mini-symposium on this subject was organized in the Dynamics Days South America 2010 Conference. The main goal of this mini-symposium was to present recent developments in both fundamental aspects and dynamical analysis of turbulence in nonlinear waves and fusion plasmas. In this paper we present a summary of the works presented at this mini-symposium. Among the questions to be addressed were the onset and control of turbulence and spatio-temporal chaos.     

Synthesis of Cu-TiNT,characterization, and antibacterial properties evaluation

Copper ion–exchanged titanate nanotubes (Cu-TiNTs) had been prepared from a simple ion-exchange reaction between copper salt and sodium titanate nanotubes (Na-TiNT) which was synthesized by alkaline hydrothermal synthesis starting from titanium oxide of anatase phase. A thorough structural and morphological characterization of Cu-TiNT (and Na-TiNT) was done by using various material characterization techniques, such as X-ray diffraction, Raman spectroscopy, energy-dispersive X-ray spectroscopy, and transmission electron microscopy to reveal retention of tubular structure of titanate nanotubes with decoration of copper (II) oxide on the surface of the tubes as well as an exchange of Na⁺ ion by Cu²⁺ ion in the interlamellar space. The antibacterial properties of the Cu-TiNT were evaluated by broth macrodilution method using microtiter trays, with concentration ranging between 512 and 0.5 μg/mL. The Cu-TiNT demonstrated no clinically relevant antibacterial activity alone (minimum inhibitory concentration ≥ 1024 μg/mL), but when associated with gentamicin, this compound enhanced the antibiotic activity of this drugs against strains of Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli. The results were very promising to the utilization of the Cu-TiNT as an adjuvant to the antibiotic therapy.     

Photolumiscent Properties of Nanorods and Nanoplates Y<Subscript>2</Subscript>O<Subscript>3</Subscript>:Eu<Superscript>3+</Superscript>

Nanorods and nanoplates of Y₂O₃:Eu³⁺ powders were synthesized through the thermal decomposition of the Y(OH)₃ precursors using a microwave-hydrothermal method in a very short reaction time. These powders were analyzed by X-ray diffraction, field emission scanning electron microscopy, Fourrier transform Raman, as well as photoluminescence measurements. Based on these results, these materials presented nanoplates and nanorods morphologies. The broad emission band between 300 and 440 nm ascribed to the photoluminescence of Y₂O₃ matrix shifts as the procedure used in the microwave-hydrothermal assisted method changes in the Y₂O₃:Eu³⁺ samples. The presence of Eu³⁺ and the hydrothermal treatment time are responsible for the band shifts in Y₂O₃:Eu³⁺ powders, since in the pure Y₂O₃ matrix this behavior was not observed. Y₂O₃:Eu³⁺ powders also show the characteristic Eu³⁺ emission lines at 580, 591, 610, 651 and 695 nm, when excited at 393 nm. The most intense band at 610 nm is responsible for the Eu³⁺ red emission in these materials, and the Eu³⁺ lifetime for this transition presented a slight increase as the time used in the microwave-hydrothermal assisted method increases.     

Stille cross‐coupling reaction using Pd/BaSO4 as catalyst reservoir

Stille cross‐coupling reactions between iodobenzene and tributylphenyltin were carried out in ethanol/water solution using different amounts of Pd/BaSO₄ as catalyst reservoir in a ligand‐free system and high yields were obtained. Other substituted biaryls were obtained with good yields. The catalyst can be reused up to three times with some loss in activity. Filtration of the catalyst and product extraction yielded a solution that kept its activity, showing the presence of Pd(0)/Pd(II) species that can be regarded as the true catalysts. Interestingly, both 2‐bromotiophene and chlorobenzene yielded the desired corresponding reaction products. Copyright © 2007 John Wiley & Sons, Ltd.