Molecular Engineering of Trigonal Octupolar Materials Based on 2,4,6-Diarylamino-1,3,5-Triazines

Molecular engineering of some 2,4,6-(substituted biarylamino)-1,3,5-triazines and crystal data belonging to the products 2,4,6-(m,m’-ditolylamino)-1,3,5-triazine, 2,4,6-(p,p’-ditolylamino)-1,3,5-triazine and 2,4,6-(phenyl-p-tolylamino)-1,3,5-triazine were reported. Retrosynthetic analysis of trigonal octupolar networks led to the identification of tris-substituted diarylamino-triazines as molecular analogs of Piedfort units formed by cofacial dimers of 2,4,6-triaryloxy-1,3,5-triazine molecules. Synthesis of mono and diarylamiono triazines is achieved by coupling of the corresponding anilines with cyanuric chloride. Synthesis of diarylamines exhibiting different functional groups on two phenyl rings is attempted; the successful attempt in the case of phenyl-p-tolylamine is described. All the crystals obtained so far belong to centrosymmetric space group P21/c. Though none of the molecules retain trigonal symmetry in the crystal structures, pseudo-trigonal assembly of molecules is identified in some cases. The assembly of molecules within the crystals results in columnar structures formed by C-H..N and C-H..pi interactions

A class of sulfonamides as carbonic anhydrase I and II inhibitors

<p>Four groups of novel sulfonamide derivatives: (i) acetoxybenzamide, (ii) triacetoxybenzamide, (iii) hydroxybenzamide and (iv) trihydroxybenzamide, all having thiazole, pyrimidine, pyridine, isoxazole and thiadiazole moieties were prepared and their inhibitory effects were studied on two metalloenzymes, i.e. carbonic anhydrase isozymes (hCA I and II), purified from human erythrocyte cells by Sepharose-4B-l-tyrosine-sulfanilamide affinity chromatography. These enzymes are present in almost all living organisms to catalyse the synthesis of bicarbonate ion (HCO₃⁻) from carbon dioxide and water. The sulfonamide derivatives were found to be active against hCA I and II in the range of 2.62–136.54 and 5.74–210.58 nM, respectively.</p

Gas chromatography-isotope dilution mass spectrometry method validation for target pesticides in soybeans

The production of certified reference materials requires the application of highly accurate methods for characterisation. A gas chromatography-isotope dilution mass spectrometry method, setting ambitious performance criteria, was developed for eight selected pesticides in soybeans. Pressurised liquid extraction was followed by automated gel-permeation chromatography and solid-phase extraction clean-up. Pesticides identification respected a Commission Decision and guidelines of the Directorate General for Health and Food Safety (DG SANTE). Reliable quantification involved stable isotopically labelled analogues as internal standards. Validation, according to ISO/IEC 17,025 and DG SANTE guidelines, assessed linearity, LOD/LOQ, trueness, selectivity, precision, stability and robustness. Mean recoveries ranges (83–109%, relative standard deviations < 3%), repeatability (2.2–4.8%), day-to-day variation (0.6–4.2%) and combined uncertainty (1.2–4.2%) were fit for purpose. The method is highly accurate and suitable for certification of the selected pesticides in soybean matrix reference material.JRC.F.6-Reference Material

Preparation of a Tc-99m-labeled graft polymer and its in vitro and in vivo evaluation

The aim of this study is the synthesis of a novel Tc-99m-labeld graft polymer and the biological evaluation of its in vitro and in vivo properties. To this end, a L-proline-graft-poly(HEMA) was prepared and labeled with Tc-99m. The radiochemical yield of approximately the Tc-99m-labeled compound amounted to 97 +/- 2.3%. The cytotoxicity test revealed no cytotoxic effect after a 24- and 48-h incubation. The results of the hemolysis test showed that hemolysis was non-toxic with an effect level of less than 2%. Subsequently, the biodistribution in healthy rats was determined. High accumulation of the polymer was observed in the pancreas, thyroid and prostate

An interlaboratory comparison on whole water samples

The European Water Framework Directive 2000/60/EC requires monitoring of organic priority pollutants in so called “whole water” samples, i.e. in aqueous non-filtered samples that contain natural colloidal and suspended particulate matter. Colloids and suspended particles in the liquid phase constitute a challenge for sample homogeneity and stability. Within the joint research project ENV08 “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive 2000/60/EC” whole water test materials were developed by spiking defined amounts of aqueous slurries of ultra-finely milled contaminated soil or sediment and aqueous solutions of humic acid into a natural mineral water matrix. This paper presents the results of an European-wide interlaboratory comparison (ILC) using this type of test materials. Target analytes were tributyl tin, polybrominated diphenyl ethers and polycyclic aromatic hydrocarbons in the ng/L concentration range. Results of the ILC indicate that the produced materials are sufficiently homogeneous and stable to serve as samples for e.g. proficiency testing or method validation. To our knowledge, this is the first time that ready to use water materials with a defined amount of suspended particulate and colloidal matter have been applied as test samples in an interlaboratory exercise. These samples meet the requirements of the European Water Framework Directive. Previous proficiency testing schemes mainly employed filtered water samples fortified with a spike of the target analyte in a water-miscible organic solvent.JRC.D.2-Standards for Innovation and sustainable Developmen

functional outcome in late adolescence/early adulthood of patients with autism spectrum disorder and its relationships with parental burnout and depression: A preliminary multi-center, cross-sectional study.

The aim of this study is to determine the functioning of adults with autism spectrum disorders (ASDs) diagnosed in childhood and depression and burnout levels among their parents. A total of 261 adults with ASDs and their parents were recruited for the study. Both parents completed the Beck Depression and Maslach Burnout Inventories and reported the functioning of their adult offspring with ASDs. Only 5.4 % of our sample reported “good” or “very good” outcomes. The most common psychiatric comorbidities were intellectual disabilities and attention-deficit/hyperactivity disorder. Maternal burnout and depression scores were significantly elevated compared to those of fathers. There is an undeniable urgent need for more research to identify the needs of adults and families suffering from ASD. Modifications for those with ASD may have to be made for support in workplaces, achieving driving licenses, using public transportation and attendance at tertiary education

Efficacy and Safety of Trastuzumab Emtansine in Her2 Positive Metastatic Breast Cancer: Real-World Experience

Aim The aim of this study is to evaluate the efficacy and toxicity of trastuzumab emtansine (T-DM1) in cases with metastatic breast cancer (mBC) in different lines of treatment. Method Retrospective analysis of T-DM1 results of human epidermal growth factor receptor 2 (Her2) positive 414 cases with mBC from 31 centers in Turkey. Findings Except 2, all of the cases were female with a median age of 47. T-DM1 had been used as second-line therapy in 37.7% of the cases and the median number of T-DM1 cycles was 9. Progression-free survival (PFS) and overall survival (OS) times were different according to the line of treatment. The median OS was found as 43, 41, 46, 23 and 17 months for 1st, 2nd, 3rd, 4th and 5th line, respectively (p = 0.032) while the median PFS was found as 37, 12, 8, 8 and 8 months, respectively (p = 0.0001). Treatment was well tolerated by the patients. The most common grade 3-4 adverse effects were thrombocytopenia (2.7%) and increased serum gamma-glutamyl transferase (2%). Discussion The best of our knowledge this is the largest real-life experience about the safety and efficacy of T-DM1 use in cases with mBC after progression of Her2 targeted treatment. This study suggests and supports that T-DM1 is more effective in earlier lines of treatment and is a reliable option for mBC