Total phenol analysis of weakly supported water using a laccase-based microband biosensor

The monitoring of phenolic compounds in wastewaters in a simple manner is of great importance for environmental control. Here, a novel screen printed laccase-based microband array for in situ, total phenol estimation in wastewaters and for water quality monitoring without additional sample pre-treatment is presented. Numerical simulations using the finite element method were utilized for the characterization of micro-scale graphite electrodes. Anodization followed by covalent modification was used for the electrode functionalization with laccase. The functionalization efficiency and the electrochemical performance in direct and catechol-mediated oxygen reduction were studied at the microband laccase electrodes and compared with macro-scale electrode structures. The reduction of the dimensions of the enzyme biosensor, when used under optimized conditions, led to a significant improvement in its analytical characteristics. The elaborated microsensor showed fast responses towards catechol additions to tap water – a weakly supported medium – characterized by a linear range from 0.2 to 10 μM, a sensitivity of 1.35 ± 0.4 A M⁻¹ cm⁻² and a dynamic range up to 43 μM. This enhanced laccase-based microsensor was used for water quality monitoring and its performance for total phenol analysis of wastewater samples from different stages of the cleaning process was compared to a standard method.     

Adaptation of Decoy Fusion Strategy for Existing Multi-Stage Search Workflows

A number of proteomic database search engines implement multi-stage strategies aiming at increasing the sensitivity of proteome analysis. These approaches often employ a subset of the original database for the secondary stage of analysis. However, if target-decoy approach (TDA) is used for false discovery rate (FDR) estimation, the multi-stage strategies may violate the underlying assumption of TDA that false matches are distributed uniformly across the target and decoy databases. This violation occurs if the numbers of target and decoy proteins selected for the second search are not equal. Here, we propose a method of decoy database generation based on the previously reported decoy fusion strategy. This method allows unbiased TDA-based FDR estimation in multi-stage searches and can be easily integrated into existing workflows utilizing popular search engines and post-search algorithms.

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Acylative kinetic resolution of racemic amines using N-phthaloyl-(S)-amino acyl chlorides

A comparative study of the kinetic resolution of racemic 2-methyl-1,2,3,4-tetrahydroquinoline and 2,3-dihydro-3-methyl-4H-1,4-benzoxazine using N-phthaloyl-(S)-amino acyl chlorides as chiral acylating agents is described. Temperature and solvent effects on the stereochemical features have been examined. It has been found that N-phthaloyl-(S)-phenylalanyl and N-phthaloyl-(S)-2-phenylglycyl chlorides bearing aromatic substituents close to the stereogenic centre are more stereoselective acylating agents than N-phthaloyl-(S)-alanyl chloride. For the preparative kinetic resolution of racemic amines N-phthaloyl-(S)-phenylalanyl chloride proved to be the most appropriate chiral acylating agent.     

Oxidative sulfamidation of vinyl silanes: A route to diverse silylated N-Heterocycles

The reaction of trimethyl(vinyl)silane 1 and dimethyl(divinyl)silane 2 with various sulfonamides in the oxidative system (tert-BuOCl + NaI) has been studied and shown to be an efficient approach for the synthesis of silylated N-heterocycles. Triflamide demonstrated the reactivity principally different from that of arenesulfonamides. With silane 1, it afforded the products of iodochlorination and bis(triflamidation) (major), whereas arenesulfonamides gave N-arenesulfonylaziridines in up to 91% yield. Silane 2 with arenesulfonamides yielded the products of mono and bis(iodochlorination), mono and bis(aziridination), and 3,5-diiodo-4,4-dimethyl-1-(arylsulfonyl)-1,4-azasilinanes. By contrast, triflamide, apart from the products of halogenation and iodotriflamidation, unexpectedly gave 3-(trifluoromethylsulfonyl)-5-(triflamido)oxazolidine as the main product. The structure of most heterocyclic products is proved by X-ray analysis. The effect of the silyl group in the substrate and of the substituent in the reagent on the course of oxidative sulfamidation is discussed by comparing with all-carbon analogues.     

“Isocyanide-less” Ugi/Intramolecular Diels-Alder reaction of 5-hydroxymethylfurfural

The one-pot, three-step, four-component Ugi-IMDAF reaction with 5-hydroxymethylfurfural provides simple access to hydroxymethyl-substituted epoxyisoindolones in a diastereoselective and stereospecific manner. The protocol avoids the transfer or isolation of isocyanides, and the broad scope was illustrated by the synthesis of 22 different compounds bearing various substituents on the heterocyclic core.     

The use of ∝-diazo-γ-butyrolactone in the Büchner-Curtius-Schlotterbeck reaction of cyclic ketones: A facile entry into spirocyclic scaffolds

The first example of the Büchner-Curtius-Schlotterbeck reaction of cyclic ketones with a stabilized cyclic diazo compound partner is described. The approach towards spirocyclic scaffolds has been exemplified with readily available ∝-diazo-γ-butyrolactone. The reaction proved to be viable with BF₃?OEt₂ as the preferred catalyst and displayed substantial sensitivity to the size of the cyclic ketone.     

Edge-defined film-fed growth of Yb:YVO4 single crystal plates

The applicability of the edge-defined film-fed growth (EFG) technique for Yb_xY_(1−x)VO₄ (x=0.05, 0.1 and 1) was approved by successful growth of crystals up to 80 mm in length as the thin plates. Low-angle grain boundaries and the crystal coloration as main defects were found. Optimal seed orientation was suggested on the strength of vanadate crystal plate morphology. Optical properties, chemical composition and the crystalline quality were investigated.     

Crystal Structure of Decakis(μ-chloro)-tetrakis(1,2,4-triphenylcyclopentadienyl)-hexakis(tetrahydrofuran)-di-potassium-tetra-neodymium(III) Tetrahydrofuran Trisolvate

Journal of Chemical Crystallography - The crystal structure of decakis(μ-chloro)-tetrakis(1,2,4-triphenylcyclopentadienyl)-hexakis(tetrahydrofuran)-di-potassium-tetra-neodymium(III)...