Monolithic metal–organic framework MIL‐53(Al)‐polymethacrylate composite column for the reversed‐phase capillary liquid chromatography separation of small aromatics

A monolithic capillary column containing a composite of metal–organic framework MIL‐53(Al) incorporated into hexyl methacrylate‐co‐ethylene dimethacrylate was prepared to enhance the separation of mixtures of small aromatic compounds by using capillary liquid chromatography. The addition of 10 mg/mL MIL‐53(Al) microparticles increased the micropore content in the monolithic matrix and increased the Brunauer–Emmett–Teller surface area from 26.92 to 85.12 m²/g. The presence of 1,4‐benzenedicarboxylate moieties within the structure of MIL‐53(Al) as an organic linker greatly influenced the separation of aromatic mixtures through π–π interactions. High‐resolution separation was obtained for a series of alkylbenzenes (with resolution factors in the range 0.96–1.75) in less than 8 min, with 14 710 plates/m efficiency for propylbenzene, using a binary polar mobile phase of water/acetonitrile in isocratic mode. A reversed‐phase separation mechanism was indicated by the increased retention factor and resolution as the water percentage in the mobile phase increased. A stability study on the composite column showed excellent mechanical stability under various conditions. The higher resolution and faster separation observed at increased temperature indicated an exothermic separation, whereas the negative values for the free energy change of transfer indicated a spontaneous process.     

A facile ZrO<Subscript>2</Subscript> nanoparticles catalyzed synthesis of 2-amino-5-arylpyrimido[4,5-<Emphasis Type="Italic">b</Emphasis>]quinolinediones

In this investigation, an efficient and ecofriendly multicomponent reaction is described for the green synthesis of 2-amino-5-arylpyrimido[4,5-b]quinolinedione derivatives using ZrO₂ (NPs). In this protocol, the reaction of 2,6-diaminopyrimidin-4(1H)-one, arylaldehyde and 1,3-cyclohexanedione or 5,5-dimethyl-1,3-cyclohexanedione in the presence of ZrO₂ (NPs) in ethylene glycol at 120 °C produced the desired products in excellent yields (90–98 %) and short reaction times (8–60 min.). Use of recyclable catalyst, green solvent, easy workup and excellent yields are the notable features of this method.     

Set amenability for semigroups

In this paper a concept of amenability for an arbitrary subset A of discrete semigroup S called A-amenable is introduced and studied. This concept is characterized by several equivalent statements which are analogues of properties characterizing left amenable semigroups. We also obtain the relationship between this version of amenability and Følner’s condition.     

Preparation and chromatographic properties of a multimodal chiral stationary phase based on phenyl-carbamate-propyl-beta-CD for HPLC

A phenylcarbamate derivative of 2-hydroxypropyl-beta-CD bonded stationary phase was prepared by a previously described method. Its enantiomeric recognition abilities were evaluated as chiral stationary phase (CSP) in normal, polar organic and RP conditions by HPLC. The relevant structural features of the prepared stationary phase which make it an effective chiral selector are discussed. This material seems to have an excellent enantioselectivity for a variety of racemic analytes in the three modes. Hence it can be considered a highly effective multimodal column. Retention factor (k), selectivity (alpha) and resolution (R(s)) were the chosen parameters to describe the column performance. Optimization of these separations was discussed in terms of mobile phase composition, flow rate and structural patterns of the injected analytes.     

Sensitive analysis of amino acids with carrier-mediated single drop microextraction in-line coupled with capillary electrophoresis

In order to analyze amino acids sensitively without derivatization, we have developed carrier-mediated single drop microextraction (SDME). Nonane-1-sulfonic acid was added to an acidic sample donor solution as a carrier to form neutral ion pair complexes with amino acids. The ion pair complexes were extracted to the organic phase, covering a drop of an aqueous basic acceptor phase hanging at the tip of a capillary, and then back-extracted to the basic acceptor phase, where both the amino acids and the carrier have negative charges and the ion pair complexes are broken. The resulting extract of enriched amino acids was injected into the capillary and analyzed by capillary electrophoresis. With 20-min SDME with agitation of the donor phase, enrichment factors of four aromatic amino acids were up to 120-fold, yielding the LOD of 70-500 nM. The linear dynamic ranges for corrected peak areas were 1-100 μM with linear correlation coefficients larger than 0.9959. With internal standardization, the intraday RSDs of migration times and corrected peak areas were 0.01-0.04% and 2.0-3.7%, respectively. The capabilities of sample cleanup including desalting and preconcentration of carrier-mediated SDME were demonstrated with the analysis of human urine after minimal pretreatment of acidification and centrifugation.     

Hydrogen-bonded perylene/terthiophene-materials: synthesis and spectroscopic properties

The synthesis of layered donor/acceptor-materials based on perylenes (1a–c) and ter(thiophen)es (2a, 2b), ordered by hydrogen bonding moieties is reported. Based on the successful (selective) chlorination of 3,4:9,10-perylene tetracarboxylic dianhydride (3) to obtain a perylene derivative with only four chlorine atoms, subsequent functionalization with different hydrogen-bonding moieties is achieved via the azide/alkyne click reaction as proven by extensive ESI-TOF measurements. The perylene- (1a–c) and terthiophene- (2a, 2b) compounds are useful as acceptor and donor parts, respectively, in organic solar cells as proven via UV–vis and fluorescence measurements. Charge transfer between donor and acceptor parts (2a/1b) was determined as 41% via fluorescence resonance energy transfer (FRET), proving the association of the two components via the attached hydrogen bonding moieties. These measurements indicate that the mixture 2a/1b displays large potential for use as a layered ordered material with controlled spacings for organic solar cells based on a thereby facilitated charge-transfer.     

Determination of capsaicinoids in Capsicum species using ultra performance liquid chromatography‐mass spectrometry

In the present work, a rapid and sensitive ultra performance liquid chromatography‐mass spectrometry method has been proposed for the analysis of capsaicinoids (nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin) present in different Capsicum samples. Extraction of capsaicinoids was carried out by liquid–liquid extraction using ethanol as an extracting solvent, while the chromatographic separation was achieved by reversed phase C₁₈ column with gradient mobile phase (solvent A: acetonitrile and solvent B: water with 0.1% formic acid). Under the optimum experimental conditions, the linear ranges were 0.5–50 μg/g with correlation coefficient (r²) >0.999 for each capsaicinoids and detection limits were 0.15, 0.05, 0.06, 0.2, and 0.1 μg/g for nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin, respectively. Run‐to‐run and day‐to‐day precisions of the method with relative standard deviations <1.5% were achieved for all analyzed capsaicinoids. The robustness of the method was determined by utilizing different injection volumes of the extracts. Furthermore, to validate the system robustness, a run of high number of capsaicinoids present in different varieties of Capsicum samples was performed in this study. All the capsaicinoids were separated in a time of less than 9 min by employing the proposed method.     

On generalized m-th root finsler metrics

In this paper, we characterize locally dually flat generalized m-th root Finsler metrics. Then we find a condition under which a generalized m-th root metric is projectively related to a m-th root metric. Finally, we prove that if a generalized m-th root metric is conformal to a m-th root metric, then both of them reduce to Riemannian metrics.     

Smart photoactive soft materials for environmental cleaning and energy production through incorporation of nanophotocatalyst on polymers and textiles

Energy and environment are key issues for the sustainable development of human beings and are also the current and long‐term focuses of scientific research. New energy and environmental technologies in combination with polymer and textile science work to create many additional functions for conventional polymers and fabrics. Therefore, some novel technical polymers and textiles, such as photovoltaic and photocatalytic polymers and textiles, have begun to emerge. Generally, light‐activated chemicals, materials, or processes that are produced or enabled by light and the agent absorbing light starting a photochemical alteration in the system is nominated as photocatalyst. This review firstly introduces the different photoactive materials, their classifications, and degradation mechanism. Then, inorganic semiconductor nanoparticles were selected as the best candidate for the application in soft materials. Finally, a detailed study was provided on both preparations of photoactive soft materials using metal oxide semiconductors and their advantages and applications. This paper will be more helpful for the scientists working in the field of photoactive soft materials.     

A Chemometric Analysis of Compounds from Native New Zealand Medicinal Flora

Several hundred (396) compounds from New Zealand flora with medicinal properties were analyzed for their physicochemical properties. It was found that approximately 10 % fulfilled all the requirements to be considered to be lead‐like, over half of the compounds were deemed to be in the drug‐like space and ≈75 % were in the known drug space. These results indicate the presence of a significant proportion of compounds that are of particular interest to pursue as potential lead compounds or therapeutics. Additionally, compound classes were analyzed separately—most carbonyl‐containing compounds (aldehydes, ketones, esters and lactones), along with phenols were the most lead‐like compounds, which also displayed very good proportions in the drug‐like and known drug space. The information presented herein can be harnessed and utilized in future work, through focussing on the compounds and compound classes that exhibit high‐levels of lead‐likeness for further development.