Preparation,spectroscopic and magnetic characterization of Cu(cyclam)M(CN)<Subscript>4</Subscript> complexes exhibiting one-dimensional crystal structures (cyclam = 1,4,8,11-tetraazacyclotetradecane,M = Ni,Pd, Pt)

From the systems Cu(II)–cyclam–[M(CN)₄]^2? (cyclam = 1,4,8,11-tetraazacyclotetradecane; M = Ni, Pd, Pt), three cyanidocomplexes Cu(cyclam)M(CN)₄ [M = Ni (1), Pd (2), Pt (3)] were isolated and characterized by chemical analysis, IR and UV–VIS spectroscopy. The three compounds are isostructural, and their crystal structures are formed by quasi-linear chains exhibiting [–Cu(cyclam)–μ–NC–M(CN)₂–μ–CN–]_n composition. The Cu(II) atoms reside on centres of symmetry and are coordinated in the form of an elongated octahedron with mean equatorial Cu–N bonds of 2.015(12), 2.017(13) and 2.011(11) Å in (1), (2) and (3), respectively, and weakly N-bonded bridging cyanido ligands in the axial positions [2.5321(9) Å in (1), 2.518(2) Å in (2) and 2.549(3) Å in (3)]. Hydrogen bonds of the N–H···N_cyanido···H–N type link neighbouring chains, and a topologically square network of paramagnetic Cu(II) atoms is formed. The magnetic susceptibilities of all three complexes follow the Curie-Weiss law with a weak antiferromagnetic exchange coupling below 5 K.     

Separation,Identification, and Quantitative Analysis of the Epimers of Cefaclor by TLC-Densitometry

JPC – Journal of Planar Chromatography – Modern TLC - The epimers of cefaclor have been separated, identified, and analyzed quantitatively by TLC. The stationary phase was silica gel 60...     

ADLOC: An Aptamer‐Displacement Assay Based on Luminescent Oxygen Channeling

Functional nucleic acids, such as aptamers and allosteric ribozymes, can sense their ligands specifically, thereby undergoing structural alterations that can be converted into a detectable signal. The direct coupling of molecular recognition to signal generation enables the production of versatile reporters that can be applied as molecular probes for various purposes, including high‐throughput screening. Here we describe an unprecedented type of a nucleic acid‐based sensor system and show that it is amenable to high‐throughput screening (HTS) applications. The approach detects the displacement of an aptamer from its bound protein partner by means of luminescent oxygen channeling. In a proof‐of‐principle study we demonstrate that the format is feasible for efficient identification of small drug‐like molecules that bind to a protein target, in this case to the Sec7 domain of cytohesin. We extended the approach to a new cytohesin‐specific single chain DNA aptamer, C10.41, which exhibits a similar binding behavior to cytohesins but has the advantage of being more stable and easier to synthesize and to modify than the RNA‐aptamer M69. The results obtained with both aptamers indicate the general suitability of the aptamer‐displacement assay based on luminescent oxygen channelling (ADLOC) for HTS. We also analyzed the potential for false positive hits and identified from a library of 18 000 drug‐like small molecules two compounds as strong singlet‐oxygen quenchers. With full automation and the use of commercially available plate readers, we estimate that the ADLOC‐based assay described here could be used to screen at least 100 000 compounds per day.     

Polyaniline/Single‐Walled Carbon Nanotubes Composite Based Triglyceride Biosensor

Nanocomposite film comprising of polyaniline (PANI) and single walled carbon nanotubes (SWCNT) has been fabricated onto indium‐tin‐oxide (ITO) coated glass plate using electrophoretic technique. Co‐immobilization of glycerol dehydrogenase (GDH) and lipase (LIP) has been done via N‐ethyl‐N′‐(3‐dimethylaminopropyl) carbodiimide and N‐hydroxysuccinimide chemistry to explore its application for triglyceride (tributyrin) sensing. Response studies have been done using linear sweep voltammetry revealing that LIP‐GDH/PANI‐SWCNT‐TB/ITO bioelectrode can detect tributyrin in the range of 50 to 400 mg dL^?1 with low Michaelis–Menten constant of 1.138 mM, improved response time of 12 s, high sensitivity as 4.28×10^?4 mA mg^?1 dL and storage stability of about 13 weeks.     

A New Example of the Structure Type A2[{Z2R4}X9]: Synthesis and Crystal Structure of Na2[{(ON)Ce4}Cl9]

First single crystals of Na₂[{(ON)Ce₄}Cl₉] were obtained during synthesis attempts for the cerium nitride chloride Ce₂NCl₃(= {N₂Ce₄}Cl₆). With a molar ratio of 8:10:3 for Ce, CeCl₃ and NaN₃ along with an excess of the flux NaCl, the mixture obviously contained a small amount of CeOCl that led to the formation of quinary Na₂[{(ON)Ce₄}Cl₉]. It crystallizes in the monoclinic space group P2₁/m(no. 11) with two formula units in the unit cell with dimensions of a = 813.21(6) pm, b = 1146.13(9) pm, c = 942.86(7) pm and β = 107.504(5) °. As the dominating structural feature {ZCe₄}^9.5+ tetrahedra are fused through trans‐oriented edges to generate chains (Z = ¹/₂ O + ¹/₂ N) just as in the structurally isotypic compounds A₂[{Z₂R₄}X₉] (A = Na, K; R = Pr, Nd, Gd; X = Cl, Br; Z = O, O/N).     

The effect of meteorological parameters on radon concentration in borehole air and water

Seasonal and short term variations of ²²²Rn activity concentration in borehole air and water of the borehole drilled in cracked quartzite were studied and possible response on meteorological parameters was examined. Seasonal change of radon concentration in borehole air due to atmospheric temperature was confirmed. Short term variation of radon concentration in borehole air coincided with the atmospheric pressure changes. The strong impact of rainfall on radon concentration values was observed both in air and water environments. The decrease of radon content in borehole air and water followed radioactive decay law exclusively in spring and summer month. Contrary to borehole water, rainfall increased radon concentration in borehole air during spring and summer months only. In this paper the results from two and half years of investigation are presented.     

Electrophoretically deposited polyaniline nanotubes based film for cholesterol detection

Polyaniline nanotube (PANI-NT) based films have been fabricated onto indium-tin-oxide (ITO) coated glass plates via electrophoretic technique. These PANI-NT/ITO electrodes have been utilized for covalent immobilization of cholesterol oxidase (ChOx) using glutaraldehyde (Glu) as cross-linker. Structural, morphological and electrochemical characterization of PANI-NT/ITO electrode and ChOx/Glu/PANI-NT/ITO bioelectrode have been done using FT-IR spectroscopy, SEM, electrochemical impedance spectroscopy and cyclic voltammetry techniques. Response studies of the ChOx/Glu/PANI-NT/ITO bioelectrode have been carried out using both linear sweep voltammetry and UV-Visible spectrophotometry. The results of the biosensing studies reveal that this bioelectrode can be used to detect cholesterol in wide detection range of 25-500 mg/dL with high sensitivity of 3.36 mA mg(-1) dL and fast response time of 30 s at pH 7.4. This bioelectrode exhibits very low value of Michaelis-Menten constant of 1.18 mM indicating enhanced interactions between cholesterol and ChOx immobilized onto this nanostructured PANI matrix.     

Total nucleotide analysis of Hydra DNA and RNA by MEKC with LIF detection and 32P‐postlabeling

The model organism Hydra has been used for molecular studies for more than 20 years, however, its DNA base composition has not been determined yet. We have analyzed DNA and total RNA of the freshwater polyp Hydra magnipapillata with two independent procedures of high accuracy and sensitivity – fluorescence labeling of nucleotides followed by CE‐LIF detection and ³²P‐postlabeling. DNA of Hydra was digested either to deoxyribonucleoside‐5′‐monophosphates or deoxyribonucleoside‐3′‐monophosphates selectively conjugated with the fluorescent dye 4,4‐difluoro‐5,7‐dimethyl‐4‐bora‐3a,4a‐diaza‐s‐indacene‐3‐propionyl ethylene diamine hydrochloride (BODIPY FL EDA) separated and detected using CE‐LIF. Both versions of the assay revealed a high A+T composition of 78 and 71%, whereas total DNA methylation (5‐methyldeoxycytidine) was 2.6 and 3.1%. Total Hydra RNA showed highest base levels for guanine (33%) and a level of 1.4% for pseudouracil. All values were in good agreement with those determined by the ³²P‐postlabeling method.     

Natural radioactivity in groundwater--a review

The issue of natural radioactivity in groundwater is reviewed, with emphasis on those radioisotopes which contribute in a significant way to the overall effective dose received by members of the public due to the intake of drinking water originating from groundwater systems. The term 'natural radioactivity' is used in this context to cover all radioactivity present in the environment, including man-made (anthropogenic) radioactivity. Comprehensive discussion of radiological aspects of the presence of natural radionuclides in groundwater, including an overview of current regulations dealing with radioactivity in drinking water, is provided. The presented data indicate that thorough assessments of the committed doses resulting from the presence of natural radioactivity in groundwater are needed, particularly when such water is envisaged for regular intake by infants. They should be based on a precise determination of radioactivity concentration levels of the whole suite of radionuclides, including characterisation of their temporal variability. Equally important is a realistic assessment of water intake values for specific age groups. Only such an evaluation may provide the basis for possible remedial actions.