4,5-Dihydroisoxazole and 4,5-dihydro-1,2,4-oxadiazole derivatives from cycloaddition reactions of nitrile oxides to alkyl N-(diphenylmethylene)-α,β-dehydroamino acids

The alkyl N-(diphenylmethylene)-α,β-dehydroamino acids 1 have been submitted to 1,3-dipolar cycloadditions with nitrile oxides. The reactivity of these compounds depends on the type and on the stereochemistry of the β-substituents. With the unsubstituted terms 1a,b the reaction occurs on the C,C double bond, providing a good method for the synthesis of the 4,5-dihydroisoxazole derivatives 3a,b,c and for the gem-functionalized 4,5-dihydroisoxazoles amino carboxylic ester 5. The β-substituted compounds 1c,d,e , inert to 1,1-dimethylethylnitrile oxide, undergo the reaction to the N,C double bond, thus giving with 2a,b the 4,5-dihydro-1,2,4-oxadiazole derivatives 4. All the reactions occur with high site- and regioselectivity.     

Simultaneous Determination of Cadmium,Lead, Copper and Mercury Ions Using Organofunctionalized SBA‐15 Nanostructured Silica Modified Graphite–Polyurethane Composite Electrode

A new sensor has been developed for the simultaneous detection of cadmium, lead, copper and mercury, using differential pulse and square wave anodic stripping voltammetry (DPASV and SWASV) at a graphite–polyurethane composite electrode with SBA‐15 silica organofunctionalized with 2‐benzothiazolethiol as bulk modifier. The heavy metal ions were preconcentrated on the surface of the modified electrode at ?1.1 V vs. SCE where they complex with 2‐benzothiazolethiol and are reduced to the metals, and are then reoxidized. Optimum SWASV conditions lead to nanomolar detection limits and simultaneous determination of Cd²⁺, Pb²⁺, Cu²⁺ and Hg²⁺ in natural waters was achieved.     

Glass/PDMS hybrid microfluidic device integrating vertically aligned SWCNTs to ultrasensitive electrochemical determinations

This communication reports a promising platform for rapid, simple, direct, and ultrasensitive determination of serotonin. The method is related to integration of vertically aligned single-walled carbon nanotubes (SWCNTs) in electrochemical microfluidic devices. The required microfabrication protocol is simple and fast. In addition, the nanomaterial influenced remarkably the obtained limit-of-detection (LOD) values. Our system achieved a LOD of 0.2 nmol L(-1) for serotonin, to the best of our knowledge one of the lowest values reported in the literature.     

Fabrication of paper-based analytical devices using a PLA 3D-printed stencil for electrochemical determination of chloroquine and escitalopram

Journal of Solid State Electrochemistry - In recent years, the use of prescribed and non-prescribed drugs has increased. Therefore, advances in new technologies and sensors for detecting molecules...     

Short synthesis of tryptophane and β-carboline derivatives by reaction of indoles with N-(diphenylmethylene)-α,β-didehydroamino acid esters

The ethylaluminum dichloride catalyzed Michael-type addition of indoles 1a-h to the N-(diphenylmethylene)-α,β-didehydroamino acid esters 2a-c allows a new synthesis of β-methyltryptophanes 41,m and a new route for 1,1-diphenyl-3-carbalkoxy-1,2,3,4-tetrahydro-β-carbolines 5a-m.     

Antibiotic Detection in Urine Using Electrochemical Sensors Based on Vertically Aligned Carbon Nanotubes

A sensitive way to determine levofloxacin using a sensor based on vertical aligned carbon nanotubes is described. The morphology and the electrochemical performance of the electrodes were characterised by atomic force microscopy, cyclic voltammetry and square wave voltammetry. A scan‐rate study and electrochemical impedance spectroscopy showed that the levofloxacin oxidation product is adsorbed on the electrode surface. Differential pulse voltammetry in phosphate‐buffer solution allowed the development of a method to determine levofloxacin levels in the range of 1.0–10.0 µmol L^?1, with a detection limit of 75.2 nmol L^?1. The proposed sensor was successfully applied in the determination of levofloxacin in urine, and the obtained results were in full agreement with those from the HPLC procedure.     

Evaluation of a biosensor based on reduced graphene oxide and glucose oxidase enzyme on the monitoring of second-generation ethanol production

Journal of Solid State Electrochemistry - An easily prepared biosensor based on reduced graphene oxide (rGO) and glucose oxidase (GOx) enzyme was developed to monitor the enzymatic hydrolysis...     

Thermo-sensitive chitosan–cellulose derivative hydrogels: swelling behaviour and morphologic studies

Hydrogels are three-dimensional, hydrophilic, polymer networks that are able to imbibe large amounts of water or biological fluids, while maintaining their dimensional stability. The polymer binding might be achieved by chemical or physical interactions. Physical crosslinking of a polymer to form its hydrogel, might be accomplished either by casting-solvent evaporation (SC) method or by freeze–thaw (FT) technique. The physical hydrogels, especially the ones based on natural biopolymers, like polysaccharides, are being widely used in industry and medicine due to their favourable properties: biocompatibility; biodegradability; low toxicity and eco-friendly characteristics. Polysaccharides, like chitosan (CH) and (hydroxypropyl)methyl cellulose (HPMC) have gained great attention due to its stimuli sensitive properties: pH and temperature responsiveness, respectively. Thus, within this work we have developed physically crosslinked CH:HPMC hydrogel films, using both SC and FT techniques. The attained CH:HPMC membranes were evaluated in terms of their swelling, thermal (low critical solution temperature—LCST), structural (attenuated total reflectance Fourier transform infrared spectroscopy) and morphological (scanning electron microscopy and atomic force microscopy) properties. According to these results, the developed membranes exhibit a good miscibility between the two component biopolymers. Moreover, the CH:HPMC membranes exhibit a high swelling capacity (SW_FT = 1,172 and SW_SC = 7,323), a low surface roughness (Sq = 5.6–9.5 nm) and an elevated LCST (LCST = 85.2–87.5 °C). The stimuli sensitive behaviour makes hydrogels appealing for the design of smart devices applicable in a variety of technological fields. In our particular case, we envisage the application of such materials as active substances (moisturisers, antiperspirants and scents) delivers, into textile substrates in a controlled manner.     

A functionalized renewable carbon-based surface for sensor development

This paper describes the surface modification of glassy carbon (GC) electrodes with a bamboo-based renewable carbon (RC) before and after an acid functionalization procedure with a sulfonitric solution (1:3 HNO₃/H₂SO₄). The morphology and structural characterization indicate an increase of functional groups in the functionalized renewable carbon (RCF) surface. The enhanced electroanalytical properties of RC and RCF were evaluated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in two different setups, in the presence of the redox couple ([Fe(CN)₆]^3−/4−) and escitalopram (EST). The results revealed an enhancement for the electrochemical responses of both inorganic and organic compounds in the electrolyte. Therefore, the use of new carbon-based materials such as renewable carbon for development of electrochemical sensors brings a fresh approach to low-cost device development.