Synthesis of a novel C2-symmetric thiourea and its application in the Pd-catalyzed cross-coupling reactions with arenediazonium salts under aerobic conditions

[reaction: see text] A novel thiourea-based C2-symmetric ligand was synthesized, and its application in the palladium-catalyzed Heck and Suzuki coupling reactions of arenediazonium salts was evaluated. The reactions, which were performed at room temperature, without added base, and under aerobic conditions, produced product in 4 h with good yield. The corresponding arenediazonium salts were easily generated in one step from anilines.     

Quantitation of seven polyoxypregnane glycosides in Marsdenia tenacissima using reversed-phase high-performance liquid chromatography-evaporative light-scattering detection

A high-performance liquid chromatography coupled with an evaporative light scattering detector (HPLC-ELSD) has been developed for the simultaneous determination of seven polyoxypregnane glycosides, tenacissosides A, B, G, H, I and marsdenosides C, G, in the stem of Marsdenia tenacissima, a Chinese herbal medicine. With a C18 analytical column, the analytes were separated efficiently using methanol-water as the mobile phase in a gradient program. The method limits of detection ranged from ca. 0.3 microg for marsdenoside C to ca. 0.5 microg for marsdenoside G and the method limits of quantitation from 1.0 microg for marsdenoside C to 1.7 microg for marsdenoside G, respectively. The intra- and inter-day precisions of the method were evaluated and all were less than 4%. All the recoveries for the spiked analytes exceeded 90%. This method was successfully used to analyze 19 samples of the stem of M. tenacissima.     

A new liquid-phase microextraction method based on solidification of floating organic drop

In the present study, a new and versatile liquid-phase microextraction method is described. This method requires very simple and cheap apparatus and also a small amount of organic solvent. Eight microliters of 1-undecanol was delivered to the surface of solution containing analytes and solution was stirred for a desired time. Then sample vial was cooled by inserting it into an ice bath for 5 min. The solidified 1-undecanol was transferred into a suitable vial and immediately melted; then, 2 μL of it was injected into a gas chromatograph for analysis.Some polycyclic aromatic hydrocarbons (PAHs) were used as model compounds for developing and evaluating of the method performance. Analysis was carried out by gas chromatography/flame ionization detection (GC/FID).Several factors influencing the microextraction efficiency, such as the nature and volume of organic solvent, the temperature and volume of sample solution, stirring rate and extraction time were investigated and optimized. The applicability of the technique was evaluated by determination of trace amounts of PAHs in environmental samples. Under the optimized conditions, the detection limits (LOD) of the method were in the range of 0.07-1.67 μg L⁻¹ and relative standard deviations (R.S.D.) for 10 μg L⁻¹ PAHs were <7%. A good linearity (r² > 0.995) in a calibration range of 0.25-300.00 μg L⁻¹ was obtained. After 30 min extraction duration, enrichment factors were in the range of 594-1940. Finally, the proposed method was applied to the determination of trace amounts of PAHs in several real water samples, and satisfactory results were resulted. Since very simple devices were used, this new technique is affordable, efficient, and convenient for extraction and determination of low concentrations of PAHs in water samples.     

Soft‐Chemical Exfoliation Route to Layered Cobalt Oxide Monolayers and Its Application for Film Deposition and Nanoparticle Synthesis

A colloidal suspension of exfoliated, layered cobalt oxide nanosheets has been synthesized through the intercalation of quaternary tetramethylammonium ions into protonated lithium cobalt oxide. According to atomic force microscopy, exfoliated nanosheets of layered cobalt oxide show a plateau‐like height profile with nanometer‐level height, underscoring the formation of unilamellar 2D nanosheets. The exfoliation of layered cobalt oxide was cross‐confirmed by X‐ray diffraction, UV/Vis spectroscopy, and transmission electron microscopy. The maintenance of the hexagonal in‐plane structure of the cobalt oxide lattice after the exfoliation process was evidenced by selected‐area electron diffraction and Co K‐edge X‐ray absorption near‐edge structure analysis. The zeta‐potential measurements clearly demonstrated the negative surface charge of cobalt oxide nanosheets. Adopting the nanosheets of layered cobalt oxide as a precursor, we were able to prepare the monodisperse CoO nanocrystals with a particle size of ≈10 nm as well as the heterolayered film composed of cobalt oxide monolayer and polycation.     

A Microbial Sensor Based on Direct Electron Transfer at Shewanella Sp. Drop‐Coated Screen‐Printed Carbon Electrodes

Aerobically grown Shewanella sp. bacterial suspension drop‐coated on a disposable screen‐printed carbon electrode was found to possess electroactivity without the aid of redox mediator. Cyclic voltammetric studies revealed the characteristics of a mixed diffusion adsorption‐controlled electrochemical process for direct electron transfer at the bacteria‐modified electrode. Both FE‐SEM and ATR FT‐IR experiments were carried out to investigate the surface characteristics. The electroanalytical applicability was further demonstrated for electrocatalytic reduction of arsenite, hydrogen peroxide and nitrite. Low cost and very simple manufacturing procedure allow for the proposed bacterial sensor to be applied as disposable devices.