Development of a Sensitive LC Assay with Fluorescence Detection for the Determination of Zearalenone in Rat Serum

A simple and sensitive liquid chromatographic assay with fluorescence detection assay was developed for the determination of zearalenone levels in rat serum. The assay utilized a single liquid–liquid extraction with t-butyl methyl ether and isocratic elution using a mobile phase consisting of acetonitrile and 0.1% triethylamine in distilled water (pH = 6) (50:50, v/v). Linearity was observed over a concentration range from 10 to 1,000 ng mL^?1 (r = 0.9995), with the limit of quantification at 10 ng mL^?1 with 100 μL of rat serum. The validated assay was applied to a pharmacokinetic study in rats.     

Direct determination of arsine in gases by inductively coupled plasma-dynamic reaction cell-mass spectrometry

Reliable determination of arsine (AsH₃) in gases is of great importance due to stringent regulations associated with health, safety and environmental issues. It is, however, challenging for an analyst to determine trace airborne arsine concentrations without specifically designed collection procedures using adsorption, desorption, dissolution or impinging techniques. To circumvent such technical barrier, we have newly developed a direct analytical method, characterized by introduction of an arsine gas sample into stable plasma stream, followed by gas-phase oxidation of arsine with molecular oxygen in a dynamic reaction cell (DRC) equipped within the inductively coupled plasma-mass spectrometry (ICP/MS) system, followed by subsequent detection of AsO⁺ ion. This preliminary work used trace arsine concentrations (161 μg m⁻³, 322 μg m⁻³, and 645 μg m⁻³) gravimetrically prepared in N₂ balance. The proposed method was optimized for the important experimental parameters such as the flow rates of the reaction gas, the arsine sample, and the carrier gas. This method was then validated by demonstrating good figure-of-merits including the low limit of detection (0.10 μg m⁻³), good linearity (r² > 0.9915), low measurement uncertainty (0.66%), and high speed of analysis (<6 min). The proposed method is expected to be potentially applicable to the determination of arsine in real workplace air after appropriate modifications are made.     

Quantitative analysis of human serum leptin using a nanoarray protein chip based on single-molecule sandwich immunoassay

We report a method for the quantitative analysis of human serum leptin, which is a protein hormone associated with obesity, using a nanoarray protein chip based on a single-molecule sandwich immunoassay. The nanoarray patterning of a biotin-probe with a spot diameter of 150 nm on a self-assembled monolayer functionalized by MPTMS on a glass substrate was successfully accomplished using atomic force microscopy (AFM)-based dip-pen nanolithography (DPN). Unlabeled leptin protein molecules in human serum were detected based on the sandwich fluorescence immunoassay by total internal reflection fluorescence microscopy (TIRFM). The linear regression equation for leptin in the range of 100 zM-400 aM was determined to be y = 456.35x + 80,382 (R = 0.9901). The accuracy and sensitivity of the chip assay were clinically validated by comparing the leptin level in adult serum obtained by this method with those measured using the enzyme-linked immunosorbent assay (ELISA) performed with the same leptin standards and serum samples. In contrast to conventional ELISA techniques, the proposed chip methodology exhibited the advantages of ultra-sensitivity, a smaller sample volume and faster analysis time.     

Topical application of solubilized Reseda luteola extract reduces ultraviolet B-induced inflammation in vivo

We investigated the skin tolerance and anti-inflammatory potential of a nanoparticular solubilisate of a luteolin-rich Reseda extract (s-RE) in two independent studies in vivo. Reseda luteola extract containing 40% flavonoids was solubilized with polysorbate, resulting in product micelles with a diameter of 10 (±1.5) nm. Standardized inflammation was induced by irradiating test areas on the back of healthy volunteers with defined doses of ultraviolet B (UVB). In the first study different concentrations of s-RE were tested in 10 volunteers to evaluate dose-dependency of anti-inflammatory effects of s-RE. In the second randomized, double-blind, placebo-controlled study a defined concentration of s-RE (2.5% w/w) was tested in 40 volunteers in comparison to the vehicle (glycerol) and hydrocortisone (1% w/w). s-RE dose-dependently reduced UVB-induced erythema when applied 30 min before irradiation. To a lesser extent, topical application of s-RE after irradiation also reduced UVB-induced erythema. s-RE was as effective as hydrocortisone, whereas the vehicle had no effect. Occlusive application of s-RE on non-irradiated test sites did not cause any skin irritation. Due to excellent skin tolerance combined with potent anti-inflammatory properties s-RE bears potential especially for the prevention but also for the treatment of inflammatory skin conditions such as UV-induced erythema.     

Structural determination of glucosylceramides isolated from marine sponge by fast atom bombardment collision‐induced dissociation linked scan at constant B/E

Five glucosylceramides (GlcCers) were isolated by reversed phase high‐performance liquid chromatography from the MeOH extracts of a marine sponge, Haliclona (Reniera) sp., collected from the coast of Ulleung Island, Korea, and analyzed by fast atom bombardment mass spectrometry (FAB–MS) in positive‐ion mode. FAB‐mass spectra of these compounds included protonated molecules [M + H]⁺ and abundant sodiated molecules [M + Na]⁺ from a mixture of m‐NBA and NaI. The structures of these GlcCers, which were similar, were elucidated by FAB‐linked scan at constant B/E. To find diagnostic ions for their characterization, the GlcCers were analyzed by collision‐induced dissociation (CID) linked scan at constant B/E. The CID‐linked scan at constant B/E of [M + H]⁺ and [M + Na]⁺ precursor ions resulted in the formation of numerous characteristic product ions via a series of dissociative processes. The product ions formed by charge‐remote fragmentation provided important information for the characterization of the fatty N‐acyl chain moiety and the sphingoid base, commonly referred to as the long‐chain base. The product ions at m/z 203 and 502 were diagnostic for the presence of a sodiated sugar ring and β‐D ‐glucosylsphinganine, respectively. For further confirmation of the structure of the fatty N‐acyl chain moiety in each GlcCer, fatty acid methyl esters were obtained from the five GlcCers by methanolysis and analyzed by FAB–MS in positive‐ion mode. On the basis of these dissociation patterns, the structures of the five GlcCers from marine sponge were elucidated. In addition, the accurate mass measurement was performed to obtain the elemental composition of the GlcCers isolated from marine sponge. Copyright © 2009 John Wiley & Sons, Ltd.     

Mesoporous TiO2 nano networks: Anode for high power lithium battery applications

Anatase phase mesoporous TiO₂ with I41/amd space group was synthesized via the urea assisted hydrothermal method. The existence of mono phasic TiO₂ sub-microspheres of uniform particle size (ca. 400 nm) encompassing an average crystallite size of 14 nm was demonstrated using the XRD, FE-SEM and TEM analysis. Surface area of ca. 116.49 m²/g along with a pore size of 7 nm was calculated using the BET and adsorption isotherm measurements which authenticated the mesoporous nature of the synthesized material. Suitable calcination temperature for the better electrochemical property was established via the optimization process. Accordingly, the mesoporous TiO₂ calcined at 400 °C displayed improved cycleability with excellent rate capability ever reported, even at 20 C-rate of discharge. The reason for the superior rate capability is corroborated to the highly mesoporous nature of the TiO₂ sub-microspheres that has imparted desirable surface area apposite for enhanced ionic and electronic diffusion.     

Capacitance response of double-walled carbon nanotubes depending on surface modification

The capacitive behaviors of high-purity double-walled carbon nanotubes (DWNTs) were investigated before and after oxidation using nitric acid (HNO₃). The electrodes prepared from the HNO₃-oxidized DWNTs have exhibited higher capacitances than the pristine nanotube electrode in both aqueous and non-aqueous systems, despite the deterioration of their specific surface area after HNO₃ oxidation. The superiority of the HNO₃-oxidized DWNTs in capacitance properties is caused by the variations of surface wettability and the interstitial pore structure of nanotube bundles, which result from the introduction of polar oxygen functional groups onto the nanotube surface by HNO₃ oxidation.     

Investigations of flow field designs in direct methanol fuel cell

An experimental and simulation research had been performed to investigate the performance as well as the flow distribution in the cathode flow field in the case of direct methanol fuel cells (DMFCs). The gas was well distributed in serpentine flow field, whereas stagnation of the gas was observed in parallel flow field. These would contribute to the cell performance greatly due to mass transfer effect when the cells start operating. In addition, the durability test of DMFC was drastically affected in parallel flow field due to poor ability to drain flooded water produced electrochemically at cathode and crossover from anode. In addition, pressure drops of different flow fields were also investigated to evaluate their contribution and feasibility as an economic application for DMFC. DMFC with serpentine flow field featuring higher pressure difference resulted in a larger parasitic energy demand. However, the optimal flow field designs are needed to balance the performance and pressure loss to achieve a uniform fluid distribution and simultaneously minimize energy demand for mass transport. Consequently, flow field with grid pattern appears to be the optimal design for the DMFC cathode.     

Inside Cover: Self‐Template‐Directed Formation of Coordination‐Polymer Hexagonal Tubes and Rings,and their Calcination to ZnO Rings (Angew. Chem. Int. Ed. 8/2009)

Hexagonal tubes and rings with unusual shapes were generated through a unique self‐template‐directed growth mechanism. As described by M. Oh and co‐workers in the Communication on page 1459 ff., initially formed solid coordination polymer particles (CPPs) act as templates for the growth of the final hexagonal tubes and rings. Simple calcination of these unusually shaped CPPs results in the spontaneous formation of ZnO particles while the unique shape is maintained.