Lifting intertwining relations

This note is devoted to the lifting problem for the intertwining relation

Fast and simple glucose assay based on filter paper as enzymes carrier using phone camera detection

Glucose is a typical diagnostic marker of diabetes mellitus but it may be also helpful during diagnosis of some types of poisoning, immunological disorder or long-term stress at hospitalized patients. Diagnosis of diabetes mellitus in time is indispensable for prevention of life-threatening complication and so, accurate and easy device for non-invasive and accurate self-diagnosis is necessary. Simple assay based on filter paper with chitosan layer and with immobilized enzymes glucose oxidase and peroxidase and phone camera detection has been proposed for home-care glucose detection in urine. Data were processed in RGB (red–green–blue) color model when blue color channel showed the best sensitivity to changing glucose concentrations. Assay exerted linear regression from 0 to 4 mmol/l and limit of detection was set to be 166 µmol/l. Assay was not influenced by any interfering substances including maltose, sucrose, sorbitol or fructose or by urine matrix substance such as bovine serum albumin, ascorbic acid, uric acid or urea. Measurement of glucose from spiked urine samples reveals also no influence of the matrix on the assay. Long-term stability was measured and filter papers coated by enzymes showed excellent stability for at least 9 weeks without any special treatment or package. In comparison with differently modified filter paper, filter paper with both chitosan and enzymes showed the best sensitivity to changing glucose concentration. In a conclusion, simple (phone camera detection) and fast (3-min reaction) assay for quantitative detection of glucose from urine was optimized.     

Effect of thermal decomposition processes on the thermal properties of carbon fiber reinforced cement composites in high-temperature range

Thermal conductivity, specific heat capacity, thermal diffusivity and linear thermal expansion coefficient of two types of carbon fiber reinforced cement composites are measured in the temperature range up to 800°C. Thermal conductivity and thermal diffusivity are also determined for the specimens exposed to thermal load up to 800°C before the measurement. Differential thermal analysis (DTA), mercury intrusion porosimetry (MIP), scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD) are utilized for the assessment of thermal decomposition processes taking place in the high temperature range under consideration. The high temperature thermal properties of the studied materials are found to be positively affected by the application of the high alumina cement and in the case of the Portland cement based composite also by using the autoclaving procedure in the production process. Also, the randomly distributed carbon fibers that can reduce the damage of the pore structure by the thermal decomposition processes are identified as a positive factor in this respect. A comparison of thermal conductivity vs. temperature curves obtained for the specimens pre-heated to different temperatures is found to be a useful tool in the identification of major dynamic effects in the specimens due to the thermal decomposition reactions. The results are in a good agreement with the DTA, MIP, SEM and XRD analyses. The character of the thermal conductivity measurements that in fact includes the effects of convection and radiation into the thermal conductivity coefficient can be beneficial for a simple assessment of the influence of the fire on a dividing structure.     

2‐Substituted dATP Derivatives as Building Blocks for Polymerase‐Catalyzed Synthesis of DNA Modified in the Minor Groove

2′‐Deoxyadenosine triphosphate (dATP) derivatives bearing diverse substituents (Cl, NH₂, CH₃, vinyl, ethynyl, and phenyl) at position 2 were prepared and tested as substrates for DNA polymerases. The 2‐phenyl‐dATP was not a substrate for DNA polymerases, but the dATPs bearing smaller substituents were good substrates in primer‐extension experiments, producing DNA substituted in the minor groove. The vinyl‐modified DNA was applied in thiol–ene addition and the ethynyl‐modified DNA was applied in a CuAAC click reaction to form DNA labelled with fluorescent dyes in the minor groove     

Evaluation of calibration data in capillary electrophoresis using artificial neural networks to increase precision of analysis

An RP-HPLC study for the pKa determination of a series of basic compounds related to caproctamine, a dibenzylaminediamide reversible inhibitor of acetylcholinesterase, is reported. The 2-substituted analogues, bearing substituents with different electronegativity, were analysed by RP-HPLC by using C18 C4 stationary phases with a mobile phase consisting of mixture of acetonitrile and triethylamine phosphate buffer (pH range comprised between 4 and 10). Typical sigmoidal curves were obtained, showing the dependence of the capacity factors upon pH. In general, the retention of the investigated basic analytes increased with increasing of the pH. The inflection point of the pH sigmoidal dependence was used for the dissociation constant determination at a fixed acetonitrile percentage. When plotting pKa vs. percent of acetonitrile in the mobile phase for two representative compounds, linear regression were obtained: the y intercept gave the aqueous pKa(w). The pKa estimation by HPLC method was found to be useful to underline the difference of benzylamine basicity produced by the ortho aromatic substituents. The variation of pKa values (6.15-7.80) within the series of compounds was correlated with the electronic properties of the ortho-substituents through the Hammett sigma parameter, whereas the ability of substituents to accept H-bond was found to play a role in determining the conformational behavior of the molecules.     

Post‐Synthesis Stabilization of Germanosilicate Zeolites ITH,IWW, and UTL by Substitution of Ge for Al

Germanosilicate zeolites often suffer from low hydrothermal stability due to the high content of Ge. Herein, we investigated the post‐synthesis introduction of Al accompanied by stabilization of selected germanosilicates by degermanation/alumination treatments. The influence of chemical composition and topology of parent germanosilicate zeolites ( ITH , IWW , and UTL ) on the post‐synthesis incorporation of Al was studied. Alumination of ITH (Si/Ge=2–13) and IWW (Si/Ge=3–7) zeolites resulted in the partial substitution of Ge for Al (up to 80 %), which was enhanced with a decrease of Ge content in the parent zeolite. In contrast, in extra‐large pore zeolite UTL (Si/Ge=4–6) the hydrolysis of the interlayer Ge?O bonds dominated over substitution. The stabilization of zeolite UTL was achieved using a novel two‐step degermanation/alumination procedure by the partial post‐synthesis substitution of Ge for Si followed by alumination. This new method of stabilization and incorporation of strong acid sites may extend the utilization of germanosilicate zeolites, which has been until now been limited.     

Double hydrophilic block copolymers with switchable secondary structure as additives for crystallization control

The synthesis and folding behavior of two different series of double hydrophilic block copolymers based on polyethyleneglycol and short acidic polypeptide blocks are described. The employment of those species in the crystallization of CaCO₃ and BaSO₄ shows that in contrast to the expectations from biomineral examples, a random conformation of the peptide is more advantageous in mineralization control than an -helical arrangement of the same chain, which is contradictory to the epitaxial adsorption model in biomineralization. Otherwise, the peptide block copolymers support formation of superstructures similar to those already reported, e.g. well-defined spherical, prolate, and dumbbell morphologies are found.     

Crystallization products of risedronate with carbohydrates and their substituted derivatives

The gastrointestinal absorption of bisphosphonates is in general only about 1%. To address this problem mixtures of risedronate monosodium salt with twelve varied sugar alcohols, furanoses, pyranoses and eight gluco-, manno- and galactopyranoside derivatives as counterions were designed in an effort to prepare co-crystals/new entities with improved intestinal absorption. Crystalline forms were generated by means of kinetically and/or thermodynamically controlled crystallization processes. One hundred and fifty-two prepared samples were screened by means of FT-NIR and FT-Raman spectroscopy. No co-crystal was prepared, but noteworthy results were obtained. A new solid phase of risedronate monosodium salt generated in the presence of phenyl-β-d-galactopyranoside under thermodynamically controlled crystallization conditions was found and also characterized using solid state NMR spectroscopy, X-ray powder diffraction and differential scanning calorimetry. This new polymorph was named as form P. Interactions between risedronate monosodium salt and both carbohydrates were confirmed by means of molecular dynamics simulation. In the present study the relationships between the chemical structures of the studied compounds required for crystalline form change are discussed.     

Atomic Force Microscopy of Novel Zeolitic Materials Prepared by Top‐Down Synthesis and ADOR Mechanism

Top‐down synthesis of 2D materials from a parent 3D zeolite with subsequent post‐synthetic modification is an interesting method for synthesis of new materials. Assembly, disassembly, organisation, reassembly (ADOR) processes towards novel materials based on the zeolite UTL are now established. Herein, we present the first study of these materials by atomic force microscopy (AFM). AFM was used to monitor the ADOR process through observation of the changes in crystal surface and step height of the products. UTL surfaces were generally complex and contained grain boundaries and low‐angle intergrowths, in addition to regular terraces. Hydrolysis of UTL to IPC‐1P did not have adverse effects on the surfaces as compared to UTL. The layers remained intact after intercalation and calcination forming novel materials IPC‐2 and IPC‐4. Measured step heights gave good correlation with the X‐ray diffraction determined d₂₀₀‐spacing in these materials. However, swelling gave rise to significant changes to the surface topography, with significantly less regular terrace shapes. The pillared material yielded the roughest surface with ill‐defined surface features. The results support a mechanism for the majority of these materials in which the UTL layers remain intact during the ADOR process as opposed to dissolving and recrystallising during each step.     

Analysis of 5-methyltetrahydrofolate in human blood, serum and urine by on-line coupling of capillary isotachophoresis and zone electrophoresis

The predominant circulating folate coenzyme in plasma/serum, 5‐methyltetrahydrofolate (5‐MTHF) was determined in human blood, serum and urine using a method based on the hyphenation of capillary ITP and zone electrophoresis. Measurements were done with a commercially available instrument for capillary isotachophoresis equipped with a column‐switching system. The choice of electrolytes was limited by the instability of 5‐MTHF and volatility of electrolytes for the potential coupling of the instrumentation with MS detector. To get an insight into the separability of individual sample components in an isotachophoretic analysis, we constructed zone existence diagrams for isotachophoretic electrolyte systems having a leading electrolyte composed of acetate and ammonium of pH 4.5 and 7.0, hydrocarbonate and ammonium, pH 7.8, chloride and ammonium, pH 5.6, and chloride and creatinine, pH 5.0, with hydroxide ion as the terminator. For isotachophoretic preseparation, the non‐volatile leading electrolyte with good buffering capacity composed of 1×10⁻² M HCl and 2.5×10⁻² M creatinine, pH 5.0, and terminating electrolyte composed of 1×10⁻² M MES was selected as the most suitable. The optimum BGE for CZE analysis from the standpoint of analyte stability, separability and volatility for MS coupling was 1×10⁻² M acetate with 3.5×10⁻² M ammonium, pH 4.5. Using this combination of electrolytes, LODs reached with optical detection at 220 nm were 1.6×10⁻⁷ M in human blood, 1.1×10⁻⁷ M in human serum and 4.7×10⁻⁶ M in human urine. Estimated content of 5‐MTHF in blood and serum samples of women following oral daily administration of 0.8 mg of folic acid was 1.2×10⁻⁵ and 5.8×10⁻⁶ M, respectively.