Simultaneous determination of cinnamaldehyde and its metabolite in rat tissues by gas chromatography–mass spectrometry

Cinnamaldehyde (CA), an active ingredient isolated from the traditional Chinese medicine Cortex Cinnamomi, has a wide range of bioactivities. To clarify the distribution characteristics of CA, a selective and sensitive method utilizing gas chromatography–mass spetrometry was initially developed for simultaneously determining the concentration of CA and its metabolite cinnamyl alcohol in rat tissues. Selected ion masses of m/z 131, 105 and 92 were chosen, and separation of the analytes was performed on a DB‐5 ms (30 m × 0.25 mm, 0.25 µm, thickness) capillary column by gas chromatography–mass spectrometry. The calibration curves demonstrated good linearity and reproducibility over the range of 20–2000 and 20–4000 ng/mL for various tissue samples. Recoveries ranged from 86.8 to 107.5%, while intra‐ and interday relative standard deviations were all <11.3%. The analysis method was successfully applied in tissue distribution studies for CA and cinnamyl alcohol. As CA and cinnamyl alcohol may inter‐convert to one another, simultaneous determination of both analytes provides a comparative and accurate data for tissue study. The concentrations of CA and cinnamyl alcohol remaining in spleen were the highest among the main organs, including heart, liver, spleen, lung, kidney and brain. In addition, there was no long‐term accumulation of CA in rat tissues. Copyright © 2014 John Wiley & Sons, Ltd.     

Simultaneous measurement of methyl tert‐butyl ether and tert‐butyl alcohol in human serum by headspace solid‐phase microextraction gas chromatography–mass spectrometry

The abundant production of methyl tert‐butyl ether (MTBE) and its widespread use have led to an increase in the potential for human exposure. This work described a simple, fast, sensitive, reliable and low‐cost method for the simultaneous measurement of MTBE and its metabolite, tert‐butyl alcohol (TBA) in human serum by headspace solid‐phase microextraction gas chromatography–mass spectrometry. Extraction conditions were optimized and 40 °C, 10 min, 250 rpm and 0.3 g NaCl for a 1 mL sample were the optimal conditions. This method showed good analytical performance in terms of sensitivity with limits of detection in serum (1 mL) of 0.03 µg/L for MTBE and 0.05 µg/L for TBA, accuracy (mean recovery values) from 75.8% to 85.8%, precision (relative standard deviations) <10% and sample stability (biodegradation) <10% after 28 days. A verification experiment proved the reproducibility and stability of this method as well. Finally the method was used to detect 212 specimens, and the internal dose levels for MTBE in human serum were presented in China. Copyright © 2015 John Wiley & Sons, Ltd.     

A novel non-invasive electrochemical biosensing device for in situ determination of the alcohol content in blood by monitoring ethanol in sweat

A non-invasive, passive and simple to use skin surface based sensing device for determining the blood's ethanol content (BAC) by monitoring transdermal alcohol concentration (TAC) is designed and developed. The proposed prototype is based on bienzyme amperometric composite biosensors that are sensitive to the variation of ethanol concentration. The prototype correlates, through previous calibration set-up, the amperometric signal generated from ethanol in sweat with its content in blood in a short period of time. The characteristics of this sensor device permit determination of the ethanol concentration in isolated and in continuous form, giving information of the BAC of a subject either in a given moment or its evolution during long periods of time (8 h). Moreover, as the measurements are performed in a biological fluid, the evaluated individual is not able to alter the result of the analysis. The maximum limit of ethanol in blood allowed by legislation is included within the linear range of the device (0.0005–0.6 g L⁻¹). Moreover, the device shows higher sensitivity than the breathalyzers marketed at the moment, allowing the monitoring of the ethanol content in blood to be obtained just 5 min after ingestion of the alcoholic drink. The comparison of the obtained results using the proposed device in the analysis of 40 volunteers with those provided by the gas chromatographic reference method for determination of BAC pointed out that there were no significant differences between both methods.     

Zinc polyoxometalate on activated carbon: an efficient catalyst for selective oxidation of alcohols with hydrogen peroxide

[PW₁₁ZnO₃₉]^5? was immobilized on activated carbon and characterized using Fourier transform infrared, X‐ray diffraction, Brunauer–Emmett–Teller and elemental analysis techniques. Effective oxidation of various alcohols with hydrogen peroxide was performed in the presence of this catalyst. Easy separation of the catalyst from the reaction mixture, cheapness, high activity and selectivity, stability as well as retained activity in subsequent catalytic cycles make this supported catalyst suitable for small‐scale synthesis. Copyright © 2015 John Wiley & Sons, Ltd.     

Tf2NH-catalyzed,highly regio-and stereo-selective synthesis of trisubstituted alkenes and indane derivatives from benzylic alcohols and alkenes

A reaction of benzylic alcohols with alkenes has been developed in the presence of bis(trifluoromethane)sulfonimide for the synthesis of trisubstituted alkenes and indane derivatives with high stereoselectivity.In general,benzylic alcohols react with 1,1-diaryl alkenes to afford trisubstituted alkenes,and the reaction with 1,2-disubstituted and trisubstituted alkenes affords indane derivatives through a [3 + 2] annulation reaction.     

Simultaneous detection of ammonia and humidity using transmission surface plasmon resonance technique

Abstract

Gas sensing by using the transmission surface plasmon resonance (T-SPR) technique was demonstrated. Polyacrylic acid (PAA)/5-nm-thick gold/40-nm-thick silver/polycarbonate grating substrate structure (Sensor A) responded to ammonia; however, it exhibited a strong humidity dependence. Polyvinyl alcohol (PVA)/5-nm-thick gold/40-nm-thick silver/polycarbonate grating substrate structure (Sensor B) as the sensing material was also prepared and it mainly responded to humidity. The T-SPR properties of Sensors A and B were observed simultaneously by a stacking arrangement that enabled us to obtain the responses by using a single spectrophotometer. The ammonia concentration under various humidity conditions could be accurately obtained by simultaneous measurement of Sensors A and B.     

Synthesis and characterization of a Ni nanoparticle stabilized on Ionic liquid‐functionalized magnetic Silica nanoparticles for tandem oxidative reaction of primary alcohols

In this research, preparation of the magnetic nanoparticle, coating by a silica shell using (3‐aminopropyl) triethoxysilane and synthesis of a novel sulfonic acid‐substituted imidazolium‐based ionic liquid onto the surface of these particles via a multi‐component reaction, is described. The functionalized nanoparticles was loaded by Ni nanoparticles and characterized by means of techniques such as XRD, FTIR, SEM, EDX, TEM, TGA and ICP‐OES. The nanostructures have spherical shapes that ranged in size from 80 to 100 nm. The catalytic activity of these nanoparticles was tested in aerobic oxidation of primary alcohols that showed good performance in the wide range of primary alcohols in water at mild reaction conditions. As a second step of this work, the tandem oxidative synthesis of alkylacrylonitriles and bisindolylmethanes were investigated using primary alcohols under oxidation conditions. This catalyst system can be recovered using external magnet and reused for five consecutive cycles without significantly less of its activity.     

Preparation and photochromic properties of pyrazolones/polyvinyl alcohol composite films

Novel photochromic composite films have been successfully fabricated by dispersing pyrazolone derivative:1,3-Diphenyl-4-(3-chlorobenzal)-5-hydroxypyrazole 4-phenylsemicarbazone (1a) into hydrosol of polyvinyl alcohol (PVA). The microstructure, photochromic behaviors and thermal bleaching properties were investigated by Raman spectroscopy, X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and ultraviolet-visible absorption spectroscopy (UV-vis). The results showed that 1a was not only blended but also well dispersed in the PVA polymer films with a suitable content of chromophore. Upon UV light irradiation, the composite films gradually changed from colorless to yellow and recovered fully to the initial state upon thermal bleaching. The time constants of photochromic reactions were almost the same as those of 1a observed in their crystalline state, indicating that the photochromic phenomenon is barely disturbed by the polymer matrix.     

Preparation,characterization and heterogeneous catalytic applications of GO/Fe3O4/HPW nanocomposite in chemoselective and green oxidation of alcohols with aqueous H2O2

Graphene oxide ‐ Fe₃O₄ ‐ NH₃⁺H₂PW₁₂O₄₀ ^‐ magnetic nanocomposite (GO/Fe₃O₄/HPW) was prepared by linking amino ‐ functionalized Fe₃O₄ nanoparticles (Fe₃O₄ ‐ NH₂) on the graphene oxide (GO), and then grafting 12 ‐ tungstophosphoric acid (H₃PW₁₂O₄₀) on the graphene oxide ‐ magnetite hybrid (GO ‐ Fe₃O₄ ‐ NH₂). The obtained GO/Fe₃O₄/HPW nanocomposite was well characterized with different techniques such as FT ‐ IR, TEM, SEM, XRD, EDX, TGA ‐ DTA, AGFM, ICP and BET measurements. The used techniques showed that the graphene oxide layers were well prepared and the various stages of preparation of the GO/Fe₃O₄/HPW nanocomposites successfully completed. This new nanocomposite displayed excellent performance as a heterogeneous catalyst in the oxidation of alcohols with H₂O₂. The as ‐ prepared GO/Fe₃O₄/HPW catalyst was more stable and recyclable at least five times without significantly reducing its catalytic activity.