Diamidopyrazoles: A New Class of Anion Receptors

The synthesis of a series of 3,5-diamidopyrazoles is reported. The anion binding properties of these systems were examined via ¹H NMR, UV/Vis and ITC titration techniques. Target compound 2a acts as a selective receptor for phosphate and sulfate anions in DMSO, whereas N-methylated 2b and the unmethylated species 4d show no appreciable binding affinity. Insights into the binding events occurring in solution came from the solid state structures of compounds 2a and 4a, 4b, and 4d, which were deduced from single crystal X-ray diffraction analyses.     

Bi2MoO6中空微球的制备及其光催化性能

基于Bi₂MoO₆与BiOI晶体结构上的相似性,设计以BiOI为自牺牲模板,通过原位转化法制备得到了Bi₂MoO₆中空微球。通过对时间演化中间产物以及不同温度下产物的物相和形貌进行分析,得出形成Bi₂MoO₆中空微球的最佳反应时间为8 h,最佳温度为120℃。对所制备的Bi₂MoO₆中空微球物相、形貌、比表面积以及光学性能进行了研究,表明Bi₂MoO₆中空微球表面较为疏松,内部为中空结构,具有较大的比表面积,为61 m²·g^-1。在可见光下,以甲基橙为降解对象,对所制备样品的光催化性能进行了评价。结果表明所制备的Bi₂MoO₆中空微球能在80 min内完全降解甲基橙,性能优于不同时间下的中间产物和片状结构Bi₂MoO₆的光催化性能,具有优越的可见光光催化性能。     

Ultrasound-assisted green synthesis of gold nanoparticles using citrus peel extract and their enhanced anti-inflammatory activity

Ultrasound and plant extract are two green approaches that have been used to synthesize gold nanoparticles (AuNPs); however, how the combination of ultrasound and citrus peel extract (CPE) affects the structure characteristics and the bioactivity of AuNPs remains unknown. Here we investigated the effects of ultrasound conditions on the particle size, stability, yield, phenolic encapsulation efficacy, and the anti-inflammatory activity of AuNPs. The results showed that temperature was positively correlated to the particle size and the anti-inflammatory activity of synthesized AuNPs. Increasing the power intensity significantly decreased the particle size, while increased the change of total phenolic content (ΔTPC) in the reaction mixture. The increase of ΔTPC caused the enhanced anti-inflammatory activity of AuNPs. The AuNPs synthesized with or without ultrasound treatment were characterized using UV–Vis, DLS, SEM, TEM, EDS, XRD, and FT-IR. The result verified the formation of negatively charged, spherical, stable, and monodispersed AuNPs. AuNPs synthesized with ultrasound (AuNPs-U) has smaller particle size (13.65 nm vs 16.80 nm), greater yield and anti-inflammatory activity (IC₅₀, 82.91 vs 157.71 μg/mL) than its non-ultrasound counterpart (AuNPs-NU). HPLC analysis showed that hesperidin was the key reductant for the synthesis of AuNPs. AuNPs-U also inhibited the mRNA and protein expression of iNOS and COX-2 in the LPS-induced Raw 264.7 cells. Our research elucidates the relationship between the reaction conditions and the structure characteristics and the anti-inflammatory activity of AuNPs synthesized using CPE with the help of ultrasound, thereafter, provides a feasible and economic way to synthesize AuNPs that can be used to ameliorate inflammation.     

Improvement of betalains stability extracted from red dragon fruit peel by ultrasound-assisted microencapsulation with maltodextrin

Natural betalains can be potential food additives because of their antioxidant activities, but they have poor thermal stability. In this study, betalains were extracted from red dragon fruit peel, and then encapsulated with maltodextrin by ultrasound method to increase the physicochemical properties of betalains microcapsules. The encapsulation efficiency of the betalains was above 79%, and the particle size and Zeta potential values were 275.46 nm and −29.01 mV, respectively. Compared to the control sample, onset temperature and DPPH free radical scavenging of betalains microcapsules under the modest ultrasound treatment (200 W, 5 min) was increased by 1.6 °C and 12.24%, respectively. This increase could be due to the ability of ultrasonification to create interactions between maltodextrin and betalains (as evidenced by FT-IR). Therefore, modest ultrasound treatment can be used for microcapsulation to improve the stability of betalains, and then expand the application of betalains in heat processed food field.     

从可溶性单源分子前驱体采用溶胶凝胶法制备ZnO/TiO2 纳米复合物

合成了单源分子前驱体Cl₂TiZn(dmae)₄ (dmae为2-二甲基乙醇胺),并以乙醇为溶剂,加入等摩尔量的水对其进行可控水解得ZnO/TiO₂纳米复合凝胶,经pH=9沉淀,在200、400和600 oC 烧结得到不同的产物T₂₀₀、T₄₀₀、T₆₀₀. XRD分析表明未烧结产物为无定形粉末并随着烧结温度升高晶型改善. ZnO呈纤锌矿结构(六方晶系),TiO₂呈板钛矿型结构(正交). BET分析和扫描电镜表明颗粒的大小随着烧结温度的提高而增加. 红外光谱证明Zn-O和Ti-O的特有的振动频率,OH基团烧结后的产物中被去掉. 所有的样品都显示良好的光催化活性, 且T₆₀₀活性最高.     

Effect of synthesis conditions on the preparation of titanium dioxides from peroxotitanate solution and their photocatalytic activity

Nanosized TiO₂ particles were prepared by the hydrothermal method from the amorphous powders which were precipitated in an aqueous peroxotitanate solution. The physical properties of the nanosized TiO₂ particles prepared were investigated. We also examined the activity of TiO₂ particles as a photocatalyst on the decomposition of orange II. The titania sol can be successfully crystallized to the anatase phase through hydrothermal aging at temperatures higher than 160°C. The particle size increases from 18 to 26 nm as the synthesis temperature increases from 140 to 200°C. Titania particles prepared at 180°C show the highest activity, and titania particles calcined at 400°C show also the highest activity on the photocatalytic decomposition of orange II.     

Analysis of octopamine in human doping control samples

The biogenic amine octopamine [4‐(2‐amino‐1‐hydroxyethyl)phenol] is prohibited in sports owing to its stimulating and performance‐enhancing properties. Adverse analytical findings in athletes' doping control samples commonly result from surreptitious applications; however, the occurrence of octopamine in nutritional supplements and in selected invertebrates as well as the assumption that its N‐methylated analog synephrine [4‐(1‐hydroxyethyl‐2‐methylamino)phenol, not banned by anti‐doping authorities but currently monitored in prevalence studies) might be converted in‐vivo into octopamine have necessitated a study to investigate the elimination of synephrine and octopamine present in over‐the‐counter products. Urine samples collected after administration of nutritional supplements containing octopamine and/or synephrine as well as urine samples collected after therapeutic application of octopamine‐ or synephrine‐containing drugs were analyzed using a validated solid‐phase extraction‐based procedure employing a weak cation exchange resin and liquid chromatographic/tandem mass spectrometric detection with electrospray ionization and multiple reaction monitoring. In the case of therapeutic octopamine application, the urinary concentration of the target compound increased from baseline levels below the lower limit of detection to 142 µg/mL, while urine samples collected after synephrine as well as dietary supplement administration did not yield any evidence for elevated renal excretion of octopamine. Copyright © 2011 John Wiley & Sons, Ltd.     

Evaluation of the suitability of low hazard surfactants for the separation of phenols and carotenoids from red‐flesh orange juice and olive mill wastewater using cloud point extraction

Natural antioxidants derived from plant sources attract considerable scientific interest. While classic extraction methods consume high volumes of toxic organic solvents, cloud point extraction requires surfactant not exceeding 15% of the waste volume. In preliminary tests, the suitability of various low hazard surfactants (Span 20, PEG 400, Tween 80 and 20) was explored for separation of phenols and carotenoids from olive mill wastewater and red‐flesh orange juice. Tween 80 showed the highest recovery and further applied to the next experiments. The most appropriate surfactant concentrations were 5% (for olive mill wastewater) and 7% (for orange juice) as indicated by recovery % and the rest cloud point extraction parameters (analyte concentration, concentration factor, and phase volume ratio). A double step CPE with 5% + 5% of Tween 80 recovered up to 94.4% of the total phenols from olive mill wastewater, while a 7% + 7% of Tween 80 recovered up to 72.4% of the total carotenoids from orange juice. Evaluation of the final effects and extraction efficiency of single and double step cloud point extraction shows that double step scheme seems to be preferable in both cases. Finally, phenols and carotenoids recovered by Tween 80 maintained high antiradical activity (DPPH test).