Determination of Dimenhydrinate Nasal Delivery System in the Blood by RP-LC

Dimenhydrinate (DM) is used therapeutically for the prevention of motion sickness associated with nausea and vomiting. The aim of this investigation is the development of a new, rapid, sensitive, simple and fully validated RP-LC procedure for the suitable assay of DM in pharmaceutical formulation applied in blood samples. The method was validated before the amount determination studies in order to confirm linearity, precision, accuracy, selectivity, determination and quantification limit and consistency. High determination coefficient (r ²  = 0.998) of the standard curve drawn in the linearity studies showed that the line equation can be used in the quantification of the DM. Literature was reviewed for the methods based on diphenhydramine (DIP), its metabolite dimenhydrinate, in the in vivo determination of dimenhydrinate amount. The most appropriate method to be used in LC was decided to be the method applied by benefitting from the fluorescence characteristic of DIP. Maximum excitation and emission wavelengths in the developed method were scanned using multiple wavelengths and, maximum excitation and emission wavelengths were found to be 215 and 300 nm, respectively. In the validation study used to prove validity of the method, determination coefficient of the developed standard curve was calculated as 0.998 (RSD %), and line equation was concluded to be appropriate for use in amount determination studies. BBS % (1.06, 1.84 %) values obtained as “<2 %” in the intra-day and inter-day precision studies proved the precision of the method. Selectivity study revealed that other materials used in the formulation did not exhibit absorbance in the same wavelengths. Detection and quantification limit were found as 1 and 5 ng mL^?1, respectively. The determination of DM plasma concentrations using the proposed and fully validated LC assay has allowed us to characterize DMPK in the sheep, as well as determine DM relative bioavailability.     

X-Ray,Gamma, and Neutron Radiation Tests on Epoxy-Ferrochromium Slag Composites by Experiments and Monte Carlo Simulations

Radiation shielding effects of ferrochromium slag loading hardened epoxy resin samples were investigated. Five different samples including different percentages of epoxy resin and ferrochromium slag were produced. X-ray, gamma ray, and neutron particle transmission experiments were performed for epoxy-ferrochromium slag composites. Also, FLUKA Monte Carlo simulations were made to obtain absorbed doses. As a result, radiation shielding performance increases with increasing ferrochromium slag additive in epoxy.     

The Synthesis and Characterization of Aryloxy-Linear Phosphazenes

The reactions of N-dichlorophosphoryl-P-trichloromonophosphazene with sodium o-methylphenoxide, sodium p-methylphenoxide, sodium f -naphthalenoxide, monosodium 4-(2-pyridylazo)resorcinol, and sodium 1-nitroso-2-naphthaleneoxide have been investigated. Experimental studies were carried out in argon atmosphere. The sodium aryloxides were prepared from naphthalene or phenol derivatives and metallic sodium. The phosphazene and phenolate or naphthaleneoxide were reacted at 0°;C and then refluxed. After the reaction products were separated by using column chromatography, the structures of the compounds were defined by elemental analysis, IR, 1 H, 13 C, 31 P NMR, and mass spectroscopy. Tetra- and pentasubstituted monophosphazenes were obtained from sodium o-methylphenoxide. Pentasubstituted derivatives also were obtained from sodium p-methylphenoxide and sodium f -naphthaleneoxide. Phosphazene or any phosphorus compound could not be isolated from the reaction of phosphazene with monosodium 4-(2-pyridylazo)resorcinol and sodium 1-nitroso-2-naphthaleneoxide.     

Synthesis and Evaluation of Thermal Properties of Fluorinated Poly(aryl ether) Dendritic Structures Based on Calix[4]arenes

By using a convergence approach two new poly(aryl ether) dendritic structures carrying 4-fluorobenzyl bromide on the surface and calix[4]arenes as a core with G1 were synthesized for the first time. Fluorinated dendritic structures are connected through ether bonds on the lower rim of the calix[4]arene unit. Its structure was determined by ¹H-NMR and elemental analysis. The thermal stabilities of fluorinated dendritic structures, based on calix[4]arenes, were investigated using thermogravimetric analysis. The activation energies and thermal degradation of the structures were calculated with the Ozawa Method.     

Copolymers of 2‐(3‐(6‐tetralino)‐3‐methyl‐1‐cyclobutyl)‐2‐Hydroxyethyl Methacrylate with Acrylonitrile and 4‐Vinylpyridine: Synthesis,Characterization, and Monomer Reactivity Ratios

The copolymerization of 2‐(3‐(6‐tetralino)‐3‐methyl‐1‐cyclobutyl)‐2‐hydroxyethyl methacrylate (TCHEMA), monomer with acrylonitrile and 4‐vinylpyridine were carried out in 1,4‐dioxane solution at 65°C using AIBN as an initiator. The copolymers were characterized by FTIR, ¹H‐NMR, and ¹³C‐NMR spectroscopic techniques. Thermal properties of the polymers were also studied by thermogravimetric analysis and differential scanning calorimetry. The copolymer compositions were determined by elemental analysis. The monomer reactivity ratios were calculated by the Fineman‐Ross and Kelen‐Tüdös method. Also, the apparent thermal decomposition activation energies were calculated by the Ozawa method with a Shimadzu TGA 50 thermogravimetric analysis thermobalance.     

Cationic dye adsorption by poly(N-isopropylacrylamide/maleic acid) copolymeric hydrogels prepared by gamma rays

N-isopropylacrylamide/maleic acid hydrogels containing different quantities of maleic acid have been synthesized with γ-radiation. The hydrogels were used in experiments on swelling, diffusion and adsorption of a cationic dye methylene blue. The diffusion of MB into the hydrogels was found to be the non-Fickian type. The factors influencing adsorption capacity of the hydrogel such as gel composition, and irradiation dose were systematically investigated. The equilibrium data for dye adsorption was better described by the Freundlich isotherm than Langmuir isotherm model. The kinetic studies showed that the pseudo-second-order kinetic model fits better than the data obtained from pseudo-first-order model.     

Comparison of two glutathione S -transferases used in capacitive biosensors for detection of heavy metals

This work describes the development of a heavy-metal biosensor based on either recombinant 6His-Tag glutathione S-transferase (GST-(His)₆) or glutathione S-transferase Theta 2-2 (GST-theta 2-2), and a capacitive transducer. The dynamic range of the pure bovine liver GST-Theta 2-2 biosensor was 1?fM to 1?mM for Zn²⁺, and 10?pM to 1?mM for Cd²⁺. The GST-(His)₆ biosensor was able to detect Zn²⁺ and Cd²⁺ in the range of 1?fM to 10?µM, and Hg²⁺ in the range of 1?fM to 10?mM. The bovine liver GST Theta 2-2 biosensor displays an increased selectivity and a wider dynamic range for Zn²⁺ compared with the GST-(His)₆ biosensor. Therefore, by using different GST isozymes, it is possible to modulate important characteristics of capacitive biosensors for the detection of heavy metals.     

Polarographic determination of herbicide thifensulfuron methyl/application to agrochemical pesticide,soil, and fruit juice

A novel, sensitive, simple, fast, and fully validated differential pulse polarographic (DPP) method for the determination of trace amounts of thifensulfuron-methyl in pesticide formulation, soil, and orange juice is reported. This procedure was based on a highly sensitive peak formed due to the reduction of thifensulfuron-methyl on a dropping mercury electrode over the pH range 1.00–10.00 in Britton–Robinson buffer. The polarographic reduction exhibits only a single peak in the pH ranges pH?≥?3.0 and pH?≤?6.0 and pH?=?10.0 located at potential values of ?1.010, ?1.350, and ?1.610?V (vs. SCE), respectively. The single peak appeared as a maximum at pH 3.0 (?1.010?V) was well resolved and suitable to be investigated for analytical use. This peak showed quantitative increments with the additions of standard thifensulfuron-methyl solution under the optimal conditions, and the cathodic peak current was linearity proportional to the thifensulfuron-methyl concentration in the range of 2?×?10^?7–5?×?10^?5?M. The limit of detection (LOD) and limit of quantification (LOQ) were obtained as 1.05?×?10^?7 and 3.50?×?10^?7?M, respectively, according to the relation k ?×?SD/b (where k?=?3 for LOD, k?=?10 for LOQ, SD is the standard deviation of the blank, and b is the slope of the calibration curve). The proposed method was applied to pesticide formulation (Harmony® Extra), and the average percentage recovery was in agreement with that obtained by the spectrophotometric comparison method, 97.82 and 102.6%, respectively. The method was extended to determination of thifensulfuron-methy in spiked soil and orange juice, showing a good reproducibility and accuracy with a relative standard deviation of 4.55 and 1.40%, and relative errors of +2.80 and +1.90%, respectively.     

A theoretical study on electronic structure and structure–activity properties of novel drug precursor 6‐acylbenzothiazolon derivatives

In this work, electronic properties and structure–activity relationship (SAR) parameters of 20 novel drug precursor 6‐acylbenzothiazolon derivatives with analgesic activity have been investigated theoretically by performing Austin Model‐1 (AM1) and DFT‐B3LYP/6‐31G (d) calculations with the aim to correlate the properties of each substance—particularly electronic properties and SAR parameters—with the biological interactions that are linked to their pharmacological effects. Their molecular properties were related to the biological activity of these drug precursor molecules. The relationship between octanol–water partition coefficient (log P) and each of the SAR parameters [E_LUMO–HOMO, molecular volume (V_m), ionization potential (IP), electron affinity, electronegativity (χ), chemical hardness (η), chemical softness (S), electrophilic index (ω), and molar refractivity] present linear correlation except for IP and χ. This result suggests that there are future prospects for designing or developing new drugs based on the correlation between the theoretically calculated parameters. According to AM1 calculation, the values of heat of formation of 6‐acylbenzothiazolon derivatives are negative (exothermic), which shows that these molecules are thermodynamically stable. E_LUMO–HOMO energy levels of the studied molecules are 4–5 eV, which also indicate that they are kinetically unstable. © 2011 Wiley Periodicals, Inc. Int J Quantum Chem, 2011     

Rapid detection of nitroaromatic and nitramine explosives on chromatographic paper and their reflectometric sensing on PVC tablets

Rapid and inexpensive sensing of explosive traces in soil and post-blast debris for environmental and criminological purposes with optical sensors has recently gained importance. The developed sensing method for nitro-aromatic and nitramine-based explosives is based on dropping an acetone solution of the analyte to an adsorbent surface, letting the solvent to dry, spraying an analytical reagent to produce a persistent spot, and indirectly measuring its reflectance by means of a miniature spectrometer. This method proved to be useful for on-site determination of nitro-aromatics (trinitrotoluene (TNT), 2,4,6-trinitrophenylmethylnitramine (tetryl) and dinitrotoluene (DNT)) and nitramines (1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX)) pre-adsorbed on a poly vinyl chloride (PVC) surface, with the use of different spray reagents for each group of explosives producing different colors. The calibration equations of the tested compounds as reflectance vs. concentration showed excellent linearity (correlation coefficient: 0.998-0.999). The linear quantification interval in terms of absolute quantity of analyte was 0.1-0.5 μg. The developed method was successfully tested for the analysis of military explosives Comp B and Octol, and was validated against high performance liquid chromatography (HPLC). The reflectometric sensing method could also be used for qualitative identification of the nitrated explosives on a chromatographic paper. The reagent-impregnated paper could also serve as sensor, enabling semi-quantitative determinations of TNT and tetryl.