Sintesi di nuovi singoli isomeri di -ciclodestrina neutri e carichi negativamente quali selettori chirali in elettroforesi capillare

In questo studio sono stati sintetizzati diversi derivati delle Ciclodestrine (CD) come singoli isomeri sia neutri che anionicamente derivatizzati utilizzando due diversi approcci sintetici uno di selettiva protezione e l'altra di selettiva attivazione dei gruppi funzionali presenti nella struttura CD

Terrestrial Laser Scanner and Close Range Photogrammetry point clouds accuracy assessment for the structure deformations monitoring

In this paper we show the results of several tests carried out using methods and instrumentation typical of an architectural survey, along with a set of metrological instrumentation, on a Reinforced Concrete (RC) beam subjected to increasing loads. The goal was to assess the accuracy in the displacements estimated by a medium quality terrestrial laser scanner (TLS) Focus 3d from Faro Technologies, and the low-cost digital camera Canon PowerShot S110 used in a Close Range Photogrammetry (CRP) survey. The software used for scan-data and point clouds processing was Reconstructor JRC Software v. 3.1.0, maintained by Gexcel Ltd, while the images processing was performed with the software Photoscan from Agisoft, which implements Structure from Motion (SfM) approach. Two processing strategies were used in the point clouds comparison: mesh2mesh and modelling the beam behavior fitting the contours of the beam with second order polynomials. Comparisons between the TLS and CRP techniques and the metrological equipment used in parallel highlighted the limits and potentialities of the two geomatic techniques used. It has been shown that modeling the behavior of the beam leads to significantly better results than using the mesh2mesh comparison. For the CRP the increase in accuracy was in the order of 40%, while for the TLS of 50%

Rational Design, Synthesis, Characterization and Evaluation of Iodinated 4,4′-Bipyridines as New Transthyretin Fibrillogenesis Inhibitors

The 3,30,5,50-tetrachloro-2-iodo-4,40-bipyridine structure is proposed as a novel chemical scaold for the design of new transthyretin (TTR) fibrillogenesis inhibitors. In the frame of a proof-of-principle exploration, four chiral 3,30,5,50-tetrachloro-2-iodo-20-substituted-4,40- bipyridines were rationally designed and prepared from a simple trihalopyridine in three steps, including a Cu-catalysed Finkelstein reaction to introduce iodine atoms on the heteroaromatic scaold, and a Pd-catalysed coupling reaction to install the 20-substituent. The corresponding racemates, along with other five chiral 4,40-bipyridines containing halogens as substituents, were enantioseparated by high-performance liquid chromatography in order to obtain pure enantiomer pairs. All stereoisomers were tested against the amyloid fibril formation (FF) of wild type (WT)-TTR and two mutant variants, V30M and Y78F, in acid mediated aggregation experiments. Among the 4,40-bipyridine derivatives, interesting inhibition activity was obtained for both enantiomers of the 3,30,5,50-tetrachloro-20-(4-hydroxyphenyl)-2-iodo-4,40-bipyridine. In silico docking studies were carried out in order to explore possible binding modes of the 4,40-bipyridine derivatives into the TTR. The gained results point out the importance of the right combination of H-bond sites and the presence of iodine as halogen-bond donor. Both experimental and theoretical evidences pave the way for the utilization of the iodinated 4,40-bipyridine core as template to design new promising inhibitors of TTR amyloidogenesis

Single-step green synthesis and characterization of gold-conjugated polyphenol nanoparticles with antioxidant and biological activities

Background: Gold nanoparticles (GNPs) are likely to provide an attractive platform for combining a variety of biophysicochemical properties into a unified nanodevice with great therapeutic potential. In this study we investigated the capabilities of three different natural polyphenols, epigallocatechin-3-gallate (EGCG), resveratrol (RSV), and fisetin (FS), to allow synergistic chemical reduction of gold salts to GNPs and stabilization in a single-step green process. Moreover, antioxidant properties of the nanosystems, as well as preliminary antiproliferative activity and apoptotic process investigation of model EGCG-GNPs on stable clones of neuroblastoma SH-SY5Y cells expressing CFP-DEVD-YFP reporter, were examined. Methods: The GNPs were characterized by physicochemical techniques, polyphenol content, and in vitro stability. The antioxidant activity of the GNPs was also determined by 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) cation (ABTS) radical-scavenging assays. Stable clones of neuronal SH-SY5Y-CFP-DEVD-YFP were generated and characterized, and cell viability after treatment with EGCG-GNPs was assessed after 72 hours through a 3(4,5-dimethylthiazol-2yl)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium assay. Activation of the apoptotic pathways was also investigated by Western blot analysis. Results: With a diameter in the size range of 10–25 nm, the obtained nanoparticles (NPs) were found to contain 2.71%, 3.23%, and 5.47% of EGCG, RSV, and FS, respectively. Nanoprototypes exhibited remarkable in vitro stability in various media, suggesting that NP surface coating with phytochemicals prevents aggregation in different simulated physiological conditions. The scavenging activities for DPPH and ABTS were highly correlated with EGCG, RSV, and FS content. Moreover, high correlation coefficients between the ABTS and DPPH values were found for the prepared nanosystems. EGCG-GNPs induce a dose-dependent reduction on SH-SY5Y-CFP-DEVD-YFP cell viability that is likely to involve the activation of the apoptotic pathways, similarly to free EGCG, as suggested by the processing of the CFP-DEVD-YFP reporter. Conclusion: These results prompted us to propose the ecofriendly synthesized EGCG-, RSV-, and FS-based nanogold conjugates as suitable carriers for bioactive polyphenols to be used for the treatment of disorders associated with oxidative stress, including neurodegenerative disorders, cardiovascular disease, and cancer.</br

Caratterizzazione via HPLC, HPLC.MS ed elettroforesi capillare di escina in soluzione standard e nell'estratto di castagne di <i>Aesculus hipocastanum</i>

L'escina è una molecola complessa di rilevante interesse farmaceutico e che viene comunemente estratta dai frutti Aesculus hipocastanum. In questo studio si è cercato di mettere a punto una tecnica analitica la più rapida possibile per la caratterizzazione e quantificazione dell'escina partendo da escina commerciale ed applicandola all'escina che si estrae dai frutti di Aesculus hipocastanum</i

Determination of 4-alkyl 2,5 dimethoxy-amphetamine derivatives by capillary electrophoresis with mass spectrometry detection from urine samples

The methylenedioxy-derivatives of amphetamine represent the largest group of designer drugs. The 4-methyl (DOM), -ethyl (DOET) and -propyl (DOPR) derivatives of 2,5-dimethoxy-amphetamine (2,5-DMA) were found to possess quite similar serotonin receptor affinities [R.A. Glennon, D.L. Doot, R. Young, Pharmacol. Biochem. Behav. 14 (1981) 287.]. This paper describes a method to screen for and quantify DOM, DOET and DOPR in urine samples, using capillary electrophoresis coupled to electrospray ionisation-mass spectrometry (CE-ESI-MS). Prior to CE-MS analysis, a simple solid-phase extraction (SPE) was used for sample cleanup. The method was validated according to international guidelines. Data for accuracy and precision were within required limits. Calibration curves were generated ranging from 10 to 1000 ng/mL and correlation coefficients always exceeded 0.996

The Use of Nadir and Oblique UAV Images for Building Knowledge

This paper focuses on the processing and study of 3D models obtained from images captured by an unmanned aerial vehicle (UAV). In particular, we wanted to study the accuracy gains achieved in the surveying and the measurement, such as height, area, and volume, of the dimensions of the buildings in the 3D models obtained with both nadir and oblique UAV flights. These latter types of flights are particularly suitable for the 3D modeling of cities or urban agglomerations, where it is important to achieve a complete building reconstruction, including façades and footprints of buildings. For this purpose, several UAV surveys with both nadir and oblique axes were performed. The nadir flight acquired images over an area of about 3.5 hectares containing 30 buildings, while the second flight, performed with both a nadir camera and an oblique camera, was conducted on a single building. The images from the flights were processed with Photoscan software by Agisoft and with Pix4D, studying their different potentialities and functionality. The results were compared with the data from the 1:2000 scale Geotopographic Database (DBGT), with the results of a Global Navigation Satellite System (GNSS) survey and with 3D model from the Terrestrial Laser Scanner (TLS) survey. The obtained results have shown that oblique UAV flights increase the achievable accuracy both in terms of the number of points in a point cloud, and in the in measurements taken on the 3D models, with respect to the limited cost, and at the increase in time for surveying and image processing

Determination of four thiophenethylamine designer drugs (2C-T-4, 2C-T-8, 2C-T-13, 2C-T-17) in human urine by capillary electrophoresis/mass spectrometry

An analytical procedure for the simultaneous determination in human urine of four thiophenethylamine designer drugs (2C-T series) is reported. The quantitative analysis was performed by capillary electrophoresis with mass spectrometric detection (CE/MS), using 2,5-dimethoxy-4-methylthiophenethylamine-D4 (2C-T-D4) as internal standard. In order to minimize interferences with matrix components and to preconcentrate target analytes, solid-phase extraction (SPE) was introduced in the method as a clean-up step. The method was validated according to international guidelines. The data for accuracy and precision were within required limits. Calibration curves were generated over the range from 10 to 500 ng mL−1 and correlation coefficients always exceeded 0.997. The method was demonstrated to be specific, sensitive, and reliable for the analysis of these derivatives in urine samples

Simultaneous determination of new thioamphetamine designer drugs in plasma by capillary electrophoresis coupled with mass spectrometry

A simple method for the simultaneous identification and quantification of four 2,5-methylenedioxy derivatives of 4-thioamphetamine (ALEPH series) in plasma samples was developed. The method consists of solid-phase extraction (SPE) using a Bond Elut C18 cartridge and capillary electrophoresis coupled with electrospray ionisation mass spectrometry (CE/ESI-MS). The SPE method used required only simple steps and provided a clean extract from which identification of each drug was feasible, even at low concentrations. The method was validated according to international guidelines. The calibration curves were linear over the concentration range of 50 to 1000 ng/mL for all drugs with correlation coefficients that exceeded 0.998. The lower limits of detection of the drugs were 23–43 ng/mL. The absolute recoveries for the drugs were 64–92% and 75–96% at concentrations of 100 and 500 ng/mL, respectively. The validation data (precision, accuracy, and recovery) show the reproducibility and selectivity of the method. This clean and simple method allows the routine detection of designer drugs such as thioamphetamines which may become a serious problem in the control of illegal drugs