Palladium- or ruthenium-catalyzed synthesis of 2-phenylindoles

Allyl α-phenyl-2-aminophenethyl carbonates undergo a smooth decarboxylation-dehydrogenation reaction to afford 2-phenylindole derivatives in acetonitrile at 80° in the presence of palladium complex as catalyst. In the reaction, the ruthenium hydride complex showed more effective catalytic activities. 2-Phenylindoles were also prepared from the corresponding α-phenyl-2-aminophenethylalcohols and allyl methyl carbonate by ruthenium-catalyzed cyclization.     

Parallel plate lens with metal hole array for terahertz wave band

Optical devices for terahertz wave band from 0.1 to 10 THz are rapidly expanding and require better designs. This paper proposes and designs a parallel plate lens with metal hole array for the terahertz wave band. The fast wave effect is due to the parallel plate. For this lens, the parallel plate spacing and hole array dimensions control the phase velocity and the focusing effect. It is not necessary to control the phase through the lens shape, which is flat, itself. The periodic analysis model extracted from the full model confirms the phase control by the metal hole array dimensions. The periodic model can be used for efficient iterative design. The full wave analysis results are also obtained by ANSYS HFSS and the focusing effect is confirmed. Phase control using both the parallel plate and the hole array enhances the focusing effect over the focusing effect controlled only by the metal hole array dimensions.     

A novel method for the direct derivatization of straight-chain aliphatic carboxylates after trapping on anion-exchange resin

A novel procedure for the characterization of traces of lipophilic straight-chain aliphatic carboxylate ions in aqueous samples is described. The carboxylates are adsorbed on an Amberlyst A26 [Cl^-] resin column. The resin is then dried and suspended in methyl iodide at room temperature. A gas Chromatographic analysis of the methyl iodide solution allows the determination of the carboxylates as their methyl esters. Full characterization of each carboxylate with an overall recovery over 84% from 1 ppm aqueous sample solutions is attained.     

Synthesis of New Functionalized Compounds Related to p-Extended Tetrathiafulvalenes with Quinonoidal Structures Bearing a Ferrocene Moiety

 A number of π-extended conjugated tetrathiafulvalene (TTF) analogues were synthesized as new π-donors, and their structures and physical properties were determined. UV/Vis spectra and cyclic voltammetry of the π-extended ferrocenyl donors were studied in comparison with ferrocene, ferrocenylquinone, and the parent donor. A three-electron redox behaviour was observed. The absorption spectrum of the new donor 16 showed a slight red-shift and a slight increase in intensity relative to the compared compounds.     

Formulation study of intravesical oxybutynin instillation solution with enhanced retention in bladder

A formulation study of intravesical oxybutynin (OB) preparations was carried out in order to improve the effectiveness in intravesical instillation therapy for spastic neurogenetic bladder. Sodium hyaluronate (HYA) was introduced to enhance the muco-adhesiveness of the instillation preparation, and the physicochemical properties of the OB formulation were evaluated in comparison with a conventional formulation containing hydroxypropylcellulose (HPC). The viscous properties and in vitro adhesiveness increased with the amount of the polymeric additives, and retention properties of OB in rabbit bladder were comparable after addition of 0.4% HYA and 1.0% HPC. HYA was able to enhance the intravesical retention properties of OB instillation solution to a lesser degree than HPC, it seemed to be a useful additive in the OB instillation due to its safety and mucosal-protective effect.     

Headspace solid-phase microextraction of cannabinoids in human head hair samples

A fast method was optimized and validated with the aim to detect cannabinoids (cannabidiol, cannabinol, and delta-9-tetrahydrocannabinol) in human head hair samples. The method was based on an initial procedure of external decontamination of hair samples (10 mg) with petroleum ether, followed by alkaline digestion and further extraction of cannabinoids by means of a headspace solid-phase microextraction technique (HS-SPME). GC-MS was used to identify and quantify the analytes in SIM mode. The LOQs and LODs obtained were 0.07 and 0.12 ng/mg, respectively, for all the studied cannabinoids. The method proved to be simple, rapid, and precise. By using the weighted least squares linear regression (weighting factor 1/x2), the accuracy of the analytical method was improved at the lower end of the calibration curve (from 0.12 to 12 ng/mg; r >0.98). Hair samples collected from eight volunteers (in-patients of a drug abuse rehabilitation clinic) were submitted to the proposed method. Detection of the drugs was observed in samples of the volunteers who reported frequent marijuana use (at least ten times a week).     

Hollow‐fiber liquid‐phase microextraction and gas chromatography‐mass spectrometry of barbiturates in whole blood samples

Here, we present a method for measuring barbiturates (butalbital, secobarbital, pentobarbital, and phenobarbital) in whole blood samples. To accomplish these measurements, analytes were extracted by means of hollow‐fiber liquid‐phase microextraction in the three‐phase mode. Hollow‐fiber pores were filled with decanol, and a solution of sodium hydroxide (pH 13) was introduced into the lumen of the fiber (acceptor phase). The fiber was submersed in the acidified blood sample, and the system was subjected to an ultrasonic bath. After a 5 min extraction, the acceptor phase was withdrawn from the fiber and dried under a nitrogen stream. The residue was reconstituted with ethyl acetate and trimethylanilinium hydroxide. An aliquot of 1.0 μL of this solution was injected into the gas chromatograph/mass spectrometer, with the derivatization reaction occurring in the hot injector port (flash methylation). The method proved to be simple and rapid, and only a small amount of organic solvent (decanol) was needed for extraction. The detection limit was 0.5 μg/mL for all the analyzed barbiturates. The calibration curves were linear over the specified range (1.0 to 10.0 μg/mL). This method was successfully applied to postmortem samples (heart blood and femoral blood) collected from three deceased persons previously exposed to barbiturates.     

Interactions of non-Abelian global strings

Non-Abelian global strings are expected to form during the chiral phase transition. They have orientational zero modes in the internal space, associated with the vector-like symmetry SU_(N)L+R$\mathit{SU}{(N)}_{\mathrm{L}+\mathrm{R}}$ broken in the presence of strings. The interaction among two parallel non-Abelian global strings is derived for general relative orientational zero modes, giving a non-Abelian generalization of the Magnus force. It is shown that when the orientations of the strings are the same, the repulsive force reaches the maximum, whereas when the relative orientation becomes the maximum, no force exists between the strings. For the Abelian case we find a finite volume correction to the known result. The marginal instability of the previously known Abelian η^′${\eta }^{\prime }$ strings is discussed.     

Synthesis,cyclic voltammetry,and UV–Vis studies of ferrocene-dithiafulvalenes as anticipated electron-donor materials

Abstract  New ferrocenyl ketones were obtained as precursors of novel π-conjugated ferrocene-dithiafulvalene (Fc-DTF) and π-extended-ferrocenedithia-fulvalenes (π-exFc-DTF) as electron-donor conducting materials from ferrocene by a direct aroylation process using the Friedel–Crafts reaction. Novel Fc-DTF conjugates were synthesized using the Wittig–Horner reaction and their structures were determined. The redox behavior of the ferrocenyl carbonyl compounds Fc-DTF and Fc-π-exDTF was investigated in comparison to the parent ferrocene by means of cyclic voltammetry. A one-electron redox behavior was observed for carbonylferrocenes as one wave potential, while a two-electron process was observed as two oxidation waves for the conjugates. Introduction of electron-withdrawing groups led to increasing E _pa values and decreasing ΔE _p values. The UV–Vis spectra of some compounds were studied in comparison with ferrocene. The absorption spectra showed a red-shift with a slight increase in the absorption intensities. Graphical abstract        

A fast and simple approach for the quantification of 40 illicit drugs,medicines, and pesticides in blood and urine samples by UHPLC‐MS/MS

A fast and simple approach to overcome challenges in emergency toxicological analysis, using ultra‐high performance liquid chromatography–tandem mass spectrometry (UHPLC‐MS/MS) has been developed, for the detection of analytes in blood and urine samples from the following drug classes: analgesics, benzodiazepines, antidepressants, anticonvulsants, drugs of abuse, and pesticides. These substances are relevant in the context of emergency toxicology in Brazil. The sample preparation procedure was relatively easy and fast to perform. The method was fully validated giving limits of in the range of 0.5 and 20 ng mL^?1 for blood and urine samples. The intraday and interday precision and accuracy were considered adequate for all analytes once the relative standard deviation (RSD) (%) was lower than 20% for quality control (QC) low and lower than 15% for CQ medium and high. The developed method was successfully applied to 320 real samples collected at the Poison Control Center of São Paulo, and 89.1% have shown to be positive for some of the analytes. This confirms its applicability and importance to emergency toxicological analysis, and it could be very useful in both fields of clinical and forensic toxicology.