Small-angle neutron scattering of mixed ionic perfluoropolyether micellar solutions

Aqueous mixed micellar solutions of perfluoropolyether carboxylic salts with ammonium counterions have been studied by small-angle neutron scattering. Two surfactants differing in the tail length were mixed in proportions n2/n3 = 60/40 w/w, where n2 and n3 are the surfactants with two and three perfluoroisopropoxy units in the tail, respectively. The tails are chlorine-terminated. The mixed micellar solutions, in the concentration range 0.1-0.2 M and thermal interval 20-40 degrees C, show structural characteristics of the interfacial shell that are very similar to ammonium n2 micellar solutions previously investigated; thus, the physics of the interfacial region is dominated by the polar head and counterion. The shape and dimensions of the micelles are influenced by the presence of the n3 surfactant, whose chain length in the micelle is 2 A longer than that of the n2 surfactant. The n3 surfactant favors the ellipsoidal shape in the concentration range 0.1-0.2 M with a 1/2 ionization degree of n2 micelles. The very low surface charge of the mixed micelles is attributed to the increase in hydrophobic interactions between the surfactant tails, due to the longer n3 surfactant molecules in micelles. The closer packing of the tails decreases the micellar curvature and the repulsions between the polar heads, by surface charge neutralization of counterions migrating from the Gouy-Chapman diffuse layer, leading to micellar growth in ellipsoids with greater axial ratios.     

Thalidomide analogs from diamines: Synthesis and evaluation as inhibitors of TNF-alpha production

Fourteen thalidomide analogs bearing two phthalimido units were prepared in high yields (83-94%) by condensation of different diamines with phthalic or 3-nitrophthalic anhydride. An in vitro investigation of the compounds as inhibitors of the TNF-alpha production was performed. The inhibition was higher for compounds bearing amino and nitro groups and was modulated by increasing the size of the spacers between the phthalimide groups.     

Comparison of chemical properties of food products processed by conventional and ohmic heating

The effect of ohmic and conventional heat processing of different food products on their chemical and physical parameters was studied. Depending on the food being analysed, parameters such as pH, total solids, ash, titratable acidity, ascorbic acid, total sugars, total fatty acids, total phenolic compounds, and anthocyanins content were determined before and after ohmic and conventional pasteurization techniques and the results were compared using one-way analysis of variance. In goat milk samples treated by ohmic technology the pH value (6.58) and total fatty acids content in milk fat (86.5 mass %) were comparable to those found in milk treated by conventional process, however, ohmically treated samples presented a lower content of lactic acid, 0.13 %. In cloudberry jam samples treated by ohmic technology the results of some of the main parameters tested, such as total sugar content 46.1 mass %, ascorbic acid content 2.83 mass %, and titratable acidity 6.01 mass % (as citric acid) did not show significant differences when compared with samples treated by conventional technology. Presented at the 33rd International Conference of the Slovak Society of Chemical Engineering, Tatranské Matliare, 22–26 May 2006.     

Use of cetyltrimethylammonium bromide as surfactant for the determination of copper and chromium in gasoline emulsions by electrothermal atomic absorption spectrometry

In this work, the use of cetyltrimethylammonium bromide as surfactant for the preparation of oil-in-water emulsions for the determination of Cu and Cr in gasoline by electrothermal atomic absorption spectrometry (ET AAS) was evaluated. The surfactant amount was tested in the range of 25 to 300 mg, added to 2 ml of gasoline, and completed to 10 mL with 0.1% (v/v) nitric acid solution. 150 mg of surfactant was found optimum, and a sonication time of 10 min sufficient to form an oil-in-water emulsion that was stable for several hours. The ET AAS temperature program was established based on pyrolysis and atomization curves. The pyrolysis temperatures were set at 700 and 1300 °C for Cu and Cr, respectively and the selected atomization temperatures were 2400 and 2500 °C. The time and temperature of the drying stage and the atomization time were experimentally tested to provide optimum conditions. The limits of detection were found to be 5 μg L^− 1 and 1.5 μg L^− 1 for Cu and Cr, respectively in the original gasoline samples. The relative standard deviation (RSD) ranged from 4 to 9% in oil-in-water emulsions spiked with 5 μg L^− 1 and 15 μg L^− 1 of each metal, respectively. Recoveries varied from 90 to 98%. The accuracy of the proposed method was tested by an alternate procedure using complete evaporation of the gasoline sample. The method was adequate for the determination of Cu and Cr in gasoline samples collected from different gas stations in Salvador, BA, Brazil.     

Novel Bisphosphonates Derived from 1H‐Indazole, 1H‐Pyrazolo[3,4‐b]Pyridine,and 1H‐Pyrazolo[3,4‐b]Quinoline

Novel tetraethyl ethylene‐1,1‐bisphosphonate esters derived from 1H‐indazole, 1H‐pyrazolo[3,4‐b]pyridine, and 1H‐pyrazolo[3,4‐b]quinoline were synthesized by a Michael addition reaction of tetraethyl ethylidene‐1,1‐bisphosphonate with the corresponding heterocycle, using conventional heating and microwave‐assisted methods. The microwave‐assisted method provides shorter reaction times and better yields. The hydrolysis of bisphosphonates afforded the corresponding bisphosphonic acids or salt, using concentrated hydrochloric acid or TMSBr/collidine, respectively. All new compounds were fully characterized, and their structures were assigned using ¹H, ³¹P, and ¹³C NMR and IR spectroscopies and mass spectrometry. The molecular structure of compound 6 was confirmed by X‐ray diffraction studies.     

A simple method for extracting both active oily and water soluble extract (WSE) from Nigella sativa (L.) seeds using a single solvent system

The current study provides a way of extraction for both active NSO and WSE from Nigella sativa seeds using 98% methanol. About 1?kg of ground seeds was macerated by 1:2.5 w/v (g/mL) for 72?hours. After rotary evaporation and 7 days of continuous drying and chilling at 50 and 4?°C, NSO and WSE were obtained at the same instant. Solubility tests of 24 solvents and 11 thin layer chromatographic analyses while 2, 2-diphenyl-1-picrylhydrazyl free radical scavenging assay of NSO (73.66) , WSE (33.32) and NSO?+?WSE (78.22) against ascorbic acid (IC50?=?4.28?mg/mL) was performed. WSE was found to be highly soluble in water and 5% NaOH exhibiting the same Rf value of 0.95 for EtOH:DMSO (9:1) against the honey. WSE has revealed more than twofold higher anti-oxidant activity than others. Formulation of WSE with Tualang honey may provide better targeted hydrophilic drug delivery systems.     

New designs for inhibitors of the NF-κB: DNA binding

We present a series of new inhibitors of the association between nuclear factor kappa B (NF-B) and the corresponding B site in DNA. They were designed using the lead compound 15-deoxy-^12,14 -prostaglandin J₂ (PGJ2), which is a natural product with demonstrated inhibitory efficiency for this system. First, the binding mode of PGJ2 to NF-B was unraveled by GOLD docking calculation. Subsequently, substitutions were made to PGJ2 to optimize its association with NF-B. Care was taken not to strongly increase the reactivity of the new compounds, and to keep the overall shape, size and hydrophilicity of the lead compound, which should render them a similar bioavailability. Molecular mechanics calculations were performed to decide on the suitability of the substitutions, and to evaluate the energies of association with NF-B. Density functional theory calculations were performed also to study the overall reactivity of the substituted drugs towards NF-B. Important general conclusions were obtained, concerning the improvement of these natural inhibitors; namely, a set of rational methodologies were deduced to improve the association between the PGJ2 derivatives and NF-B, and their efficiency demonstrated by generating a set of substituted complexes, some of them with a very much increased affinity for NF-B, opening new doors to enlarge the therapeutic capabilities of this class of drugs.     

高聚合度Ⅱ-型聚磷酸铵的合成

用聚合反应-热处理两段工艺合成了高聚合度的聚磷酸铵（APP）阻燃材料,其结构经XRD,粒度及平均聚合度表征。优化反应条件为：磷酸氢二铵1mol,n（磷酸氢二铵）：n（五氧化二磷）：n（脲）：1．0：1．0：0．3．干燥氨气氛下于290℃反应30min,再经250℃-280℃后处理100min-110min。APP的平均聚合度大于150,粒度小于50μm。     

Multifunctional natural fibers: the potential of core shell MgO–SiO2 nanoparticles

Cellulose - Core–shell nanoparticles (NPs) based on metal oxides, namely magnesium oxide (MgO) and silica (SiO2), are a fantastic alternative for natural fibers’ functionalization. In...     

Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization

A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min^?1 flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i‐propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min^?1 flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols.