Comprehensive two-dimensional gas chromatography with flow modulator coupled via tube plasma ionization to an atmospheric pressure high-resolution mass spectrometer for the analysis of vermouth volatile profile.

The analysis of complex samples is a big analytical challenge due to the vast number of compounds present in these samples as well as the influence matrix components could cause in the methodology. In this way, comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC × GC-MS) is a very powerful tool to achieve the characterization of complex samples. Nevertheless, due to possible coelutions occurring in these matrices, mixed spectra are generally obtained with electron ionization (EI) which could extremely complicate the identification of the analytes. Thereby, new methodology setups are required to improve the confidence on the identification in non-targeted determinations. Here, we present a high-throughput methodology consisting of GC × GC with flow modulation coupled to high-resolution atmospheric pressure mass spectrometry (HRMS) via a novel tube plasma ion source (TPI). The flow modulator allows to easily automate the GC × GC method compared to traditional cryo-modulators, while the soft ionization provided by TPI helps to preserve the [M]+• or [M+H]+ ions, thus increasing the confidence in the identification. Additionally, the combination of a flow modulation with an atmospheric pressure mass spectrometer significantly improves the sensitivity over flow modulated GC × GC-EI-MS methods because no split is required. This methodology was applied to the analysis of a complex sample such as vermouth where the volatile profile is usually considered by consumers as a product quality indicator since it raises the first sensations produced during its consumption. Using this approach, different classes of compounds were tentatively identified in the sample, including monoterpenes, terpenoids, sesquiterpenoids and carboxylic acid, and carboxylate esters among others, showing the great potential of a GC × GC-TPI-qTOF-MS platform for improving the confidence of the identifications in non-targeted applications.

Production and Characterization of Bioplastic by Polyhydroxybutyrate Accumulating Erythrobacter aquimaris Isolated from Mangrove Rhizosphere.

The synthesis of bioplastic from marine microbes has a great attendance in the realm of biotechnological applications for sustainable eco-management. This study aims to isolate novel strains of poly-ß-hydroxybutyrate (PHB)-producing bacteria from the mangrove rhizosphere, Red Sea, Saudi Arabia, and to characterize the extracted polymer. The efficient marine bacterial isolates were identified by the phylogenetic analysis of the 16S rRNA genes as Tamlana crocina, Bacillus aquimaris, Erythrobacter aquimaris, and Halomonas halophila. The optimization of PHB accumulation by E. aquimaris was achieved at 120 h, pH 8.0, 35 °C, and 2% NaCl, using glucose and peptone as the best carbon and nitrogen sources at a C:N ratio of 9.2:1. The characterization of the extracted biopolymer by Fourier-transform infrared spectroscopy (FTIR), Nuclear magnetic resonance (NMR), and Gas chromatography-mass spectrometry (GC-MS) proves the presence of hydroxyl, methyl, methylene, methine, and ester carbonyl groups, as well as derivative products of butanoic acid, that confirmed the structure of the polymer as PHB. This is the first report on E. aquimaris as a PHB producer, which promoted the hypothesis that marine rhizospheric bacteria were a new area of research for the production of biopolymers of commercial value.

Instant and quantitative epoxidation of styrene under ambient conditions over a nickel(ii)dibenzotetramethyltetraaza[14]annulene complex immobilized on amino-functionalized SBA-15.

Nickel(ii)dibenzotetramethyltetraaza[14]annulene complex (Nitmtaa) was synthetized and immobilized on post amino-functionalized SBA-15 (N-SBA-15) to obtain a stable and reusable nanocatalyst named as Nitmtaa@N-SBA-15. Here (3-aminopropyl)triethoxysilane (APTES) was first grafted on the surface SBA-15, then Nitmtaa was added and coordinated on the silica surface via APTES amine groups. The structure and morphology, and thermal stability of the prepared nanocatalyst was investigated using SEM, HR-TEM, BET, FT-IR, powder XRD, and TGA. HR-TEM and XRD results revealed a high dispersion of Nitmtaa on the SBA-15 surface. The catalytic activity of this nanocatalyst was evaluated in the epoxidation of styrene, under ambient conditions, using meta-chloroperoxybenzoic acid (m-CPBA) as the oxygen donor. This nanocatalyst showed an immediate and quantitative epoxidation of styrene with high turn-over-frequency ∼31.58 s-1. Moreover, the superior catalytic activity and high stability of Nitmtaa@N-SBA-15 could be maintained after four successive cycles. A possible reaction mechanism is also proposed.

Solvent-free hydrogenation of cyclohexene over Rh-TUD-1 at ambient conditions.

Rhodium nanoparticles (≈3-5 nm) were incorporated into the 3D mesoporous TUD-1 material by using sol-gel technique. The prepared catalyst shows high activity in the liquid phase conversion of cyclohexene to cyclohexane at room temperature (298 K), 1 atm H2 pressure, and under solvent-free conditions. Rhodium nanoparticles exhibited high stability, reusability and negligible leaching.