Reactivity of triosmium clusters with 3,4-dimethyl-1-phenylphosphole and cyanoethyldi-tert-butylphosphine ligands: X-ray crystal structures of [Os3(CO)9(μ-OH)(μ-H)(η1-PhPC4H2Me2)] and [Os3(CO)11(η1- t Bu2PC2H4CN)]

Reaction of [Os₃(μ-H)₂(CO)₁₀] with 3,4-dimethyl-1-phenylphosphole in refluxing cyclohexane affords two substituted triosmium clusters: [Os₃(CO)₉(μ-H)(μ³:η¹:η¹:η²-PhPC₄H₃Me₂)] (1) and [Os₃(CO)₉(H)(μ²-η¹:η²-PhPC₄H₄Me₂)] (2), of which cluster 2 exhibits two chromatographically non-separable isomeric forms attributed to terminal and bridging coordination of the hydride ligand, respectively. When this reaction is performed in refluxing THF, the only product is the cluster [Os₃(CO)₉(μ-OH)(μ-H)(η¹-PhPC₄H₂Me₂)] (3). Crystallographic information obtained for cluster 3 shows the phosphole ligand occupying an equatorial position, as expected, while the OH group is asymmetrically bridging unlike previously reported similar compounds. Additionally, interaction of the labile cluster [Os₃(CO)₁₁(CH₃CN)] with cyanoethyldi-tert-butylphosphine in dichloromethane at room temperature was found to give [Os₃(CO)₁₁(η¹- ^t Bu₂PC₂H₄CN)] (4) as the only product; its crystallographic characterization shows that the phosphine ligand coordinates by means of the phosphorus atom in an equatorial fashion, analogous to compound 3.     

Desorption of Coffee Pulp Used as an Adsorbent Material for Cr(III and VI) Ions in Synthetic Wastewater: A Preliminary Study

Some of the diverse agro-industrial waste generated in primary or secondary stages have proved to be promising biomaterials for treating aqueous effluents contaminated, in this case, with heavy metals. Therefore, it is necessary to know their optimal operating conditions and the regeneration or reusability of the solid by-product, an aspect related to desorption. Considering the above, this article presents the findings of a preliminary study related to the desorption process of coffee pulp without physicochemical modification (Castilla variety), an agricultural waste used as a sorbent of Cr(III and VI) ions in synthetic wastewater. The desorption efficiency of four eluting agents at defined concentrations (0.10M)—HC1, HNO₃, H₂SO₄, and EDTA—was evaluated in a time interval of 1 to 9 days. Likewise, the proposals for the sorption and/or desorption mechanisms proposed and reported in the literature with respect to the use of biosorbents derived from the coffee crop are presented. With respect to the results, the coffee pulp used in previous studies of the adsorption of chromium species mentioned (optimal conditions in synthetic water of particle size 180 μm, dose 20 g·L⁻¹, agitation 100 RPM, room temperature, time of 90 to 105 min) showed efficiencies in the removal of Cr(III) and Cr(VI) of 93.26% and 74.80%, respectively. Regarding the extracting substances used, H₂SO₄ 0.10 M was the one that presented the highest desorption percentage in both chromic species, with a desorption of 45.75% Cr(VI) and 66.84% Cr(III) in periods of 5 and 9 days, respectively, with agitation of 100 RPM and room temperature. Finally, the dissemination of preliminary results on the desorption of coffee pulp contaminated with chromic species without physicochemical modification is novel in this study, as similar work with this specific material has not yet been reported in the literature. On the other hand, the limitations of the study and future research are related to the evaluation at different concentrations and of other extractor solutions that allow improving the efficiency of desorption of these chemical species in a shorter time from the coffee pulp (with and without modification) as well as the reuse cycles. As a result, the desorption of coffee pulp used as an adsorbent material in real water could help researchers identify the possible interfering factors that affect the process (foreign anions and cations, organic matter, environmental conditions, among others).     

Pentacyclic Triterpene Profile and Its Biosynthetic Pathway in Cecropia telenitida as a Prospective Dietary Supplement

Promising research over the past decades has shown that some types of pentacyclic triterpenes (PTs) are associated with the prevention of type 2 diabetes (T2D), especially those found in foods. The most abundant edible sources of PTs are those belonging to the ursane and oleanane scaffold. The principal finding is that Cecropia telenitida contains abundant oleanane and ursane PT types with similar oxygenation patterns to those found in food matrices. We studied the compositional profile of a rich PT fraction (DE16-R) and carried out a viability test over different cell lines. The biosynthetic pathway connected to the isolated PTs in C. telenitida offers a specific medicinal benefit related to the modulation of T2D. This current study suggests that this plant can assemble isobaric, positional isomers or epimeric PT. Ursane or oleanane scaffolds with the same oxygenation pattern are always shared by the PTs in C. telenitida, as demonstrated by its biosynthetic pathway. Local communities have long used this plant in traditional medicine, and humans have consumed ursane and oleanane PTs in fruits since ancient times, two key points we believe useful in considering the medicinal benefits of C. telenitida and explaining how a group of molecules sharing a closely related scaffold can express effectiveness.     

Sodium quantitation in soft drinks: A rapid methodology by qNMR

High sodium dietary intake has a positive association with an increase in blood pressure and can be correlated with risk factors of disease. Considering that the World Health Organization recommends a sodium intake lower than 2 g day^-1 for adults, the hidden sodium content in processed foods is an important factor that compromises the assessment of a healthy diet. Accordingly, the present paper aimed to quantitate the sodium content of conventional soft drinks and their diet versions using nuclear magnetic resonance spectroscopy as a quantitative analytical technique (²³Na qNMR). The results show one free sodium signal (Na⁺) displayed as a singlet at 0 ppm in the ²³Na NMR spectrum, making its quantitation highly specific. This signal alone was used to directly determine the concentration of sodium in soft drinks. Flame photometry analysis was used to validate the method, and an excellent linearity was found in qNMR analysis (r = 0.9994) in comparison with flame photometry (r = 0.9958). In addition, a good correlation was found between sodium concentrations obtained by ²³Na NMR and flame photometry in the evaluated commercial soft drinks. Since the intensity of the resonance line is directly proportional to the number of nuclei (spins), the concentration of sodium in soft drinks can be determined via this straightforward method without the need for external calibration. The experimental acquisitions are fast (approximately 15 min), allowing the analysis of several samples in a short period of time. This is a novel alternative for sodium quantitation using an efficient NMR methodology.