Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction‐Gas Chromatography‐Mass Spectrometry

Seven monoterpenes in 4 aromatic plants (sage, cardamom, lavender, and rosemary) were quantified in liquid extracts and directly in solid samples by means of dynamic headspace‐gas chromatography‐mass spectrometry (DHS‐GC‐MS) and multiple headspace extraction‐gas chromatography‐mass spectrometry (MHSE), respectively. The monoterpenes were 1st extracted by means of supercritical fluid extraction (SFE) and analyzed by an optimized DHS‐GC‐MS. The optimization of the dynamic extraction step and the desorption/cryo‐focusing step were tackled independently by experimental design assays. The best working conditions were set at 30 °C for the incubation temperature, 5 min of incubation time, and 40 mL of purge volume for the dynamic extraction step of these bioactive molecules. The conditions of the desorption/cryo‐trapping step from the Tenax TA trap were set at follows: the temperature was increased from 30 to 300 °C at 150 °C/min, although the cryo‐trapping was maintained at ?70 °C. In order to estimate the efficiency of the SFE process, the analysis of monoterpenes in the 4 aromatic plants was directly carried out by means of MHSE because it did not require any sample preparation. Good linearity (r² > 0.99) and reproducibility (relative standard deviation % <12) was obtained for solid and liquid quantification approaches, in the ranges of 0.5 to 200 ng and 10 to 500 ng/mL, respectively. The developed methods were applied to analyze the concentration of 7 monoterpenes in aromatic plants obtaining concentrations in the range of 2 to 6000 ng/g and 0.25 to 110 μg/mg, respectively.     

Profile of TREM2-Derived circRNA and mRNA Variants in the Entorhinal Cortex of Alzheimer’s Disease Patients

Genetic variants in TREM2, a microglia-related gene, are well-known risk factors for Alzheimer’s disease (AD). Here, we report that TREM2 originates from circular RNAs (circRNAs), a novel class of non-coding RNAs characterized by a covalent and stable closed-loop structure. First, divergent primers were designed to amplify circRNAs by RT-PCR, which were further assessed by Sanger sequencing. Then, additional primer sets were used to confirm back-splicing junctions. In addition, HMC3 cells were used to assess the microglial expression of circTREM2s. Three candidate circTREM2s were identified in control and AD human entorhinal samples. One of the circRNAs, circTREM2_1, was consistently amplified by all divergent primer sets in control and AD entorhinal cortex samples as well as in HMC3 cells. In AD cases, a moderate negative correlation (r = −0.434) was found between the global average area of Aβ deposits in the entorhinal cortex and circTREM2_1 expression level. In addition, by bioinformatics tools, a total of 16 miRNAs were predicted to join with circTREM2s. Finally, TREM2 mRNA corresponding to four isoforms was profiled by RT-qPCR. TREM2 mRNA levels were found elevated in entorhinal samples of AD patients with low or intermediate ABC scores compared to controls. To sum up, a novel circRNA derived from the TREM2 gene, circTREM2_1, has been identified in the human entorhinal cortex and TREM2 mRNA expression has been detected to increase in AD compared to controls. Unraveling the molecular genetics of the TREM2 gene may help to better know the innate immune response in AD.     

Relating cyclic voltammetry and impedance analysis in a viologen electrochromic device

Viologens are electrochromic materials that have a wide range of coloration depending on the radical substituents. The results for a new blue viologen-based device, that has recently been patented, with an active area of 8.5 cm² is presented in this paper. The characterization techniques used are based on optical measurements, chronoamperometry, cyclic voltammetry, and impedance spectroscopy analysis. A study of the results obtained from these measurements provides both an overview of the reactions taking place and has allowed an equivalent circuit to be developed which relates the different electrochemical parameters. The transmittance is observed to change from 80% to 15% in 600 nm for input voltages ranging from 0 to 2.5 V. However, increasing voltage beyond 1.8 V shows no optical change, thus, maintaining the voltage below this level optimizes the use of electrical current. Voltages and charges used for each redox reaction have been computed and are seen to be linearly related. The equivalent circuit generated to mimic the process has included parameters based on Warburg diffusion and double-layer capacitances. Results from this model are consistent with measurements for up to 1.8 V. Saturation of reduced species has been deduced for input voltages beyond this level.     

Orange to black electrochromic behaviour in poly(2-(2-thienyl)-1H-pyrrole) thin films

We have studied an electrochromic precursor, 2-(2-thienyl)-1H-pyrrole (1), using two improved procedures of the Trofimov reaction. Optimised stereochemical calculations at the B3LYP/6-311G* level showed almost equal s-cis and s-trans conformational populations in 1 with marked out-of-plane deviations of ca. 30°. Model calculations suggest that the predominant rotational conformation in undoped poly(1) would be s-trans with the essential out-of-plane deviations around the all three interheterocyclic bonds of ca. 25-30°. Monomer 1 exhibited two irreversible oxidation processes at +0.86 and +1.3 V corresponding to the oxidation of the pyrrole and thiophene rings, respectively. Orange to black electrochromic behaviour was found in ClO₄⁻ doped poly(1) thin films with colouring and bleaching times of 1.8 and 1.3 s, respectively. The colouration efficiency during the bleaching process was 233 cm²/C. The optical contrast at 450 nm was 19% and in the near-IR was 36%. The band-gap of poly(1) (1.6-1.7 eV) was found to be significantly lower than that of polypyrrole (2.85 eV) and polythiophene (2.3 eV) as a consequence of increased electron delocalisation in the system. Important differences in the morphology of doped and dedoped poly(1) films were observed by atomic-force microscopy (AFM). Doped poly(1) films showed a granular morphology with primary particles of 45-60 nm in size and an average surface roughness of 3.5 nm. On the other hand, dedoped poly(1) films showed interconnected aggregates of 65-90 nm in size as a consequence of particle fusion, with a surface roughness of 9.2 nm. In summary, poly(1) is a promising material for emerging flexible electrochromic devices such as displays and variable optical attenuators.     

Laser sintered ceramic coatings of PZT nanoparticles deposited by Inkjet Printing on metallic and ceramic substrates

Lead zirconate titanate (PZT) Pb(ZrxTi1-x)O₃ is one of the most studied perovskite type ferroelectric materials due to its excellent dielectric, piezoelectric and ferroelectric properties. PZT particles and a PZT precursor were synthesized using a chemical method. A vehicle was added to the synthesized particles and precursor for obtaining two inks with appropriate rheological properties to be printed by Inkjet Printing. The use of an 80?µm diameter nozzle made necessary the utilization of an energetic ball milling for assuring the dispersion of small PZT particles in the ink. After ball milling nanoparticles of 150?nm diameter were obtained. These inks were deposited on alumina and steel substrates followed by sintering using a pulsed laser of 1064?nm wavelength. The work shows the effect laser sintering has on, both inks, the one containing PZT nanoparticles and that one based on the PZT precursor. Laser processing was optimized in order to generate suitable films to be subsequently poled. The effect of poling on these films was also studied and their piezoelectric properties were measured by a compression test. The microstructural characteristics of these films were obtained by SEM and X ray diffractometry.     

Gender-Dependent Deregulation of Linear and Circular RNA Variants of HOMER1 in the Entorhinal Cortex of Alzheimer’s Disease

The HOMER1 gene is involved in synaptic plasticity, learning and memory. Recent studies show that circular RNA derived from HOMER1 (circHOMER1) expression is altered in some Alzheimer’s disease (AD) brain regions. In addition, HOMER1 messenger (mRNA) levels have been associated with β-Amyloid (Aβ) deposits in brain cortical regions. Our aim was to measure the expression levels of HOMER1 circRNAs and their linear forms in the human AD entorhinal cortex. First, we showed downregulation of HOMER1B/C and HOMER1A mRNA and hsa_circ_0006916 and hsa_circ_0073127 levels in AD female cases compared to controls by RT-qPCR. A positive correlation was observed between HOMER1B/C, HOMER1A mRNA, and hsa_circ_0073128 with HOMER1B/C protein only in females. Global average area of Aβ deposits in entorhinal cortex samples was negatively correlated with HOMER1B/C, HOMER1A mRNA, and hsa_circ_0073127 in both genders. Furthermore, no differences in DNA methylation were found in two regions of HOMER1 promoter between AD cases and controls. To sum up, we demonstrate that linear and circular RNA variants of HOMER1 are downregulated in the entorhinal cortex of female patients with AD. These results add to the notion that HOMER1 and its circular forms could be playing a female-specific role in the pathogenesis of AD.     

All-plastic electrochromic devices based on PEDOT as switchable optical attenuator in the near IR

Advanced materials for IR applications such as thermal control in spacecraft applications or variable optical attenuators which could replace the present systems have been sought. The use of electrochromic devices based on conducting polymers will add lightness and flexibility to the final device in order to overcome the limitations of the present materials used in IR applications. In this work, we present a new all-plastic electrochromic device with optical contrast (%ΔT) of 44% at 1971 nm in the IR region based on PEDOT formulations and ionic liquid blends as electrolytes. The switching time of the device is in the order of a few seconds, with a t_c 2.7 s and t_b 3.8 s.     

Highly transparent electrochromic plastic device that changes to purple and to blue by increasing the potential

We report the assembly and characterization of a highly transparent electrochromic device showing dual-coloration (purple and blue color change) using an innovative electrochromic formulation recently patented. This electrochromic formulation is composed of the three electroactive materials needed in a traditional electrochromic device (electrolyte, electrochromic and ion storage material) embedded in a polymeric matrix to reduce the chance of device malfunction by leaking and evaporation of the solvent. Two materials based on viologen, which show different electrochromic behaviors at 1.5 and 2.5 V, have been incorporated into the electrochromic formulation. Therefore, the electrochromic device was transparent in the bleach state but depending on the potential applied the final coloration was pink at 1.5 V and blue at 2.5 V. The maximum transparency of the device was 80% in the bleach state, 25.21% at 1.5 V when showing purple coloration and 3% at 2.5 V when showing blue coloration. The device presented a coloration efficiency (CE) of 136.6 cm²/C and a coloring time of 6.5 s to achieve 90% of the maximum change in absorbance. The device exhibited a memory effect of 8 min estimated as the time needed to obtain the initial transparency.     

Optimization of Supercritical Fluid Consecutive Extractions of Fatty Acids and Polyphenols from Vitis Vinifera Grape Wastes

In this study, supercritical fluid extraction has been successfully applied to a sequential fractionation of fatty acids and polyphenols from wine wastes (2 different vitis vinifera grapes). To this aim, in a 1st step just fatty acids were extracted and in a 2nd one the polyphenols. The variables that affected to the extraction efficiency were separately optimized in both steps following an experimental design approach. The effect of extraction temperature flow, pressure, and time were thoroughly evaluated for the extraction of fatty acids, whereas the addition of methanol was also considered in the case of the polyphenols extraction. A quantitative extraction with high efficiency was achieved at a very short time and low temperatures. Concerning quantification, fatty acids were determined by means of gas chromatography coupled to mass spectrometry after a derivatization step, whereas the polyphenols were analyzed by means of high performance liquid chromatography coupled to tandem mass spectrometry and the Folin–Ciocalteu method.