Synthesis,molecular characterisation,and in vivo study of platinum(IV) coordination compounds against B16 mouse melanoma tumours

A novel platinum(IV) coordination compound with 6-mercaptopurine (6-Hmp) has been synthesised and characterised by IR and NMR spectroscopy. Spectroscopic parameters indicate the presence of two chelate (S-6, N-7) monodeprotonated ligands and two chloride ions in the coordination sphere of [PtCl₂(6-mp)₂] · H₂O (I). Two Pt(IV) coordination compounds, [PtCl₂(6-mp)₂] · H₂O (I) and [PtCl₄(dbtp)₂] (II), were used in the in vivo test against B16 mouse melanoma tumours. Cytotoxic activity of compound II against the tumour cells was found to be high (LC₁₀ = 2.6 μM, LC₅₀ = 17.0 μM, LC₉₀ = 58.0 μM) compared to that of cisplatin.     

Application of High Pressure-DTA for High Pressure-liquid Phase Epitaxy of Doped Mercury and Thallium HTS Formations

The fabrication method of superconducting thin films of compositions HgBa₂Ca₂Cu₃O_8+δ (Hg-1223) and Tl₂Ba₂CuO_y (2201) on single-crystalline SrTiO₃ and LaAlO₃ substrates is reported. The highest obtained T _c was 134 K and J _c over 10⁶ A cm^–2 at 77 K. High pressure DTA(HP-DTA) was applied to grow mercury- and thallium-based high-temperature superconducting crystals and thin films, to identify melting points of particular phases within these oxide systems and determine suitable processing conditions. The DTA system operates at the: maximum temperature of 1200°C, volume up to 5 cm³, working pressure up to 1.5 GPa and at a working atmosphere — inert gas with up to 25% oxygen. This revised version was published online in August 2006 with corrections to the Cover Date.     

Chemometric outlook on correlations between retention parameters of polar and semipolar HPLC columns and physicochemical characteristics of ampholytic substances of biological and pharmaceutical relevance

The Quantitative Property-Retention Relation (QPRR) approach was applied to analyze the correlations between the retention parameters of ampholytic, biologically active substances and their physicochemical (predicted/spectral) characteristics. The retention parameters were obtained for polar and semipolar HPLC columns at various compositions of mobile phases and pH conditions. These values are a unique collection of chromatographic parameters that are a measure of lipophilicity and, consequently, can be very helpful in assessing pharmacological potency of the compounds investigated. Three QPRR models that meet the predictive capability criteria were developed. The relationships can be used to gain pharmacologically interesting information on the biologically active ampholytic substances.

     

The influence of compression conditions on the peculiarities of self-propagating exothermal reaction in Al–Ni powder reactive materials

The paper deals with the effect of the compression conditions on the propagation front velocity of exothermal reaction and the specific heat release in Al–Ni powder reactive materials with mean particle sizes of 70–110 nm. It was shown that the velocity increases from 2.7 to 8 cm s^?1 and comes to saturation with the lowering of the porosity (η) from 0.91 to 0.34, while the dependence of the specific heat release has its maximum for η?=?0.5. The results of the X-ray diffraction analysis obtained in situ during the sample heating suggest that the sequence of phase transformations in the system does not depend on the porosity. In all cases, first in the temperature range of ~?500–540 °C the NiAl compound is formed. With the further heating up to ~?640 °C, the Ni₃Al, Ni₂Al₃ and NiAl₃ compounds are additionally formed. The calculation of kinetic parameters was performed using the obtained curves of the differential scanning calorimetry: activation energy, pre-exponential factor and reaction model. The comparison of the calculated results and the scanning electron microscopy data has shown that such behavior of the Al–Ni system with the porosity lowering occurs due to the growth of the transformation degree and is associated with the presence in the final powder mixture of mutually non-contacting Al and Ni agglomerates with the dimensions of over 10 μm.     

Kinetics and Characterization of Degradation Products of Dihydralazine and Hydrochlorothiazide in Binary Mixture by HPLC-UV,LC-DAD and LC–MS Methods

Dihydralazine and hydrochlorothiazide were stored at high temperature and humidity, under UV/Vis light and different pH, as individual drugs and the mixture. Then, a sensitive and selective HPLC-UV method was developed for simultaneous determination of dihydralazine and hydrochlorothiazide in presence of their degradation products. Finally, the degradation products were characterized through LC-DAD and LC–MS methods. Dihydralazine was sensitive to high temperature and humidity, UV/Vis light and pH?≥?7. At the same time, it was resistant to acidic conditions. Hydrochlorothiazide was sensitive to high temperature and humidity, UV/Vis light and changes in pH. Its highest level of degradation was observed in 1 M HCl. Degradation of the drugs was higher when they were stressed in the mixture. In the case of dihydralazine, the percentage degradation was 5–15 times higher. What is more, dihydralazine became sensitive to acidic conditions. Hydrochlorothiazide was shown to be more sensitive to UV/Vis light and pH?>?4. Degradation of dihydralazine and hydrochlorothiazide followed first-order kinetics. The quickest degradation of dihydralazine was found to be in 1 M NaOH while of hydrochlorothiazide was in 1 M HCl (individual hydrochlorothiazide) or at pH 7–10 (hydrochlorothiazide in the mixture). A number of new degradation products were detected and some of them were identified by our LC-DAD and LC–MS methods. In the stressed individual samples, (phenylmethyl)hydrazine and 1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide were observed for the first time. Interactions between dihydralazine and hydrochlorothiazide in the mixture were confirmed by additional degradation products, e.g., 2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1,4-trioxide.     

Close-packed monolayers of charged Janus-type nanoparticles at the air-water interface

Two DNA-block copolymers, poly(caprolactone)-DNA and poly(methyl metacrylate)-DNA, were synthesized by conjugation of a short single strand of DNA (12 or 22 mer) to a single reactive group at one end of the synthetic polymer. These polymers self-assemble in water, without the need of any cosolvent, forming micelle-like aggregates that were imaged by TEM. The solution behavior of the bioconjugated polymers was investigated by surface tension measurements. In the direction of dilution, the surface tension was measured using a down-scaled Wilhelmy plate method. To proceed in the reverse direction (concentration), we measured the surface tension of a sessile drop during its evaporation. This latter method was firstly validated using ionic and non-ionic surfactants, including polymeric surfactants. It was then applied to investigate the unimer to micelles transition of the DNA-block copolymers. In all cases, a reversible transition was observed demonstrating the existence of a critical micellar concentration, close to 0.01 mmol L⁻¹ for all the conjugates. The CMC was only slightly influenced by the length of the hydrophilic DNA block.     

Deactivation of preoxidized cobalt foil studied by CO2 pulse hydrogenation

Evolution of catalytic activity on preoxidized Co-foil in CO₂ pulse hydrogenation has been characterized. The changes in catalytic activity were not fully reversible. Possible conversion of the experimental results into one general deactivation curve was shown.