Metal Organic Framework-235 (MOF-235) Modified Carbon Paste Electrode for Catechol Determination in Water

MOF-235 is presented as an orange powder, with crystals of the octahedral formation. It was already used as adsorbent to remove different compounds from water; however, no attempts have been published about the exploration of the MOF-235 application as electrochemical sensor for organic compounds yet. MOF-235 was synthetized and after that, it was characterized by SEM, XRD and FTIR. Graphite electrodes (GEs) were modified with different MOF-235 ratio (5 %, 7 %, 10 %, 12 % and 14 %) and these modified GEs were characterized by cyclic voltammetry (CV) measurements in order to determine the effect of MOF-235 concentration on the current response. Results indicated that, a significant improvement on the current response was attained at MOF-235(10 %)/GE respect to unmodified GE. This behavior is related to the pore structure and multiple active sites on the MOF surface. The performance of the MOF-235(10 %)/GE as electrochemical sensor for detecting catechol was assessed by differential pulse voltammetry (DPV). Catechol detection response of MOF-based sensor provided a detection limit of about 12.79 μmol L⁻¹ with a correlation coefficient (R²) of about 0.9928 ranging from 12 to 514 μmol L⁻¹. Finally, MOF-235(10 %)/GE was used to determine catechol in real water matrixes.     

Study of benznidazole–cyclodextrin inclusion complexes, cytotoxicity and trypanocidal activity

The current chemotherapy for Chagas disease is still based on benznidazole, which has low solubility, but complexation with cyclodextrins provides a way of increasing the solubility. The objective of this work was to characterize the inclusion complexes formed between benznidazole (BNZ) and randomly 2-methyled-β-cyclodextrin (RM-β-CD) in aqueous solution and study cytotoxicity and trypanocidal. BNZ:RM-β-CD solution complex systems were prepared and characterized using the phase solubility diagram, nuclear magnetic resonance and a photostability assays, also to investigate the in vitro trypanocidal activity with epimastigote forms of Trypanossoma cruzi and the study of cytotoxicity against mammal cells. The phase-solubility diagram displayed an A _L-type feature, providing evidence of the formation of soluble inclusion complexes. The continuous variation method showed the existence of a complex with 1:1 stoichiometry. Toxicity assays demonstrated that inclusion complexes were able to reduce the toxic effects caused by benznidazole alone and that this did not interfere with the trypanocidal activity of the benznidazole. The use of inclusion complexes benznidazole:cyclodextrin is thus a promising alternative for the development of a safe and stable liquid formulation and a new option for the treatment of Chagas disease.     

Malva sylvestris L. extract suppresses desferrioxamine‐induced PGE2 and PGD2 release in differentiated U937 cells: the development and validation of an LC‐MS/MS method for prostaglandin quantification

Malva sylvestris is a species used worldwide as an alternative to anti‐inflammatory therapies; however, its mechanism of action remains unknown. In this paper, the anti‐inflammatory effects of M. sylvestris alcoholic extracts were evaluated by measuring the pro‐inflammatory mediators PGE₂ and PGD₂ in desferrioxamine‐stimulated phorbol 12‐myristate 13‐acetate‐differentiated U937 cells. An HPLC‐DAD fingerprint of the M. sylvestris extract was performed and caffeic acid, ferulic acid and scopoletin were identified and quantified. An HPLC‐MS/MS method was developed and validated to separate and measure the prostaglandins. The lower limits of detection (~0.5 ng/mL for PGE₂ and PGD₂) and quantification (1.0 ng/mL for PGE₂ and PGD₂) indicated that the method is highly sensitive. The calibration curves showed excellent coefficients of correlation (r > 0.99) over the range of 1.0–500.0 ng/mL, and at different levels, the accuracy ranged from 96.4 to 106.4% with an RSD < 10.0% for the precision study. This method was successfully applied using U937‐d cells. A significant dose‐dependent reduction of PGE₂ and PGD₂ levels occurred using 10 µg/mL (10.74 ± 2.86 and 9.60 ± 6.89%) and 50 µg/mL of extract (48.37 ± 3.24 and 53.06 ± 6.15%), suggesting that the anti‐inflammatory mechanisms evoked by M. sylvestris may be related to modulation of these mediators. Copyright © 2014 John Wiley & Sons, Ltd.     

Analysis of high resolution electron spin resonance spectra

Previous interpretations of the electron spin resonance spectrum of Wurster's Blue cation are shown to be incorrect. In particular the nitrogen hyperfine splitting constant previously quoted as 0·28 gauss is, in fact, 7·0 gauss. A complete analysis of the spectrum is described.     

Solid-phase extraction of triazole fungicides from water samples using disks impregnated with carbon nanotubes followed by GC-MS analysis

Triazole fungicides are pesticides widely employed in the cultivation of fruits, vegetables and grains. However, their ability to change the steroid hormone biosynthesis may result in endocrine complications for mammals, as well as changes in cholesterol and triglyceride levels and hepatotoxicity. The analysis of the triazole fungicides in superficial waters is important in order to monitor the risk for the biota. However, the use of efficient extraction procedures has been necessary in order to concentrate these pesticides before the analysis. In-disk solid-phase extraction (SPE) can be highlighted as a potential pre-concentration technique, mainly because the possibility to extract the analytes from a large sample volume, increasing the method detectability. Carbon nanotubes (CNTs) have been often used as solid extraction phase due to their high sorption capacity, surface area and internal volume, as well as mechanical, chemical and thermal stability. In this paper, we proposed the preparation of a new SPE disk impregnated with CNTs for the extraction of triazole fungicides from environmental water samples. The disks were obtained by acid corrosion of a cellulose membrane followed by its impregnation with CNTs. The developed method was validated for the analysis of triadimenol, tebuconazole and epoxiconazole, according to international validation protocols. The limits of quantification obtained for triadimenol, tebuconazole and epoxiconazole were 0.1, 0.1 and 0.05 µg L^?1, respectively. The linearity ranged from 0.05 to 10.00 µg L^?1 for epoxiconazole and from 0.1 to 10.00 µg L^?1 for triadimenol and tebuconazole, with correlation coefficients higher than 0.999 for all of them. The precisions, expressed as relative standard deviation, were lower than 12%. The accuracies were within ?12.07% to 17.7% (expressed as relative error).