Application of DSC, IST, and FTIR study in the compatibility testing of nateglinide with different pharmaceutical excipients

Experiments were done to assess the compatibility of nateglinide (NTG) with selected excipients in the development of immediate release tablets of NTG by thermal and isothermal stress testing (IST) techniques. To evaluate the drug excipient compatibility, different techniques such as differential scanning calorimetric (DSC) study, infrared (IR) spectrophotometric study, and IST were adopted. The results of DSC study showed that magnesium stearate exhibited some interaction with NTG. However, the results of IR and IST studies showed that all the excipients used in the formula were compatible with NTG. The optimized formulation developed using the compatible excipients were found to be stable after 3 months of accelerated stability studies (40 ± 2 °C and 75 ± 5% RH). Overall, compatibility of excipients with NTG was successfully evaluated using the combination of thermal and IST methods and the formulations developed using the compatible excipients was found to be stable.     

Dielectric loss,conductivity relaxation process and magnetic properties of Mg substituted Ni–Cu ferrites

The dielectric properties, dc and ac electrical resistivities of Mg substituted Ni–Cu ferrites with general formula Ni_0.5Cu_0.5−xMg_xFe₂O₄ (0.0≤x≤0.5) have been investigated as a function of frequency, temperature and composition. ac resistivity of all the samples decreases with increase in the frequency exhibiting normal ferrimagnetic behavior. The frequency dependence of dielectric loss tangent showed a maximum in between 10 Hz and 1 kHz in all the ferrites. The conductivity relaxation of the charge carriers was examined using the electrical modulus formulism, and the results indicate the presence of the non-Debye type of relaxation in the prepared ferrites. Similar values of activation energies for dc conduction and for conductivity relaxation reveal that the mechanism of electrical conduction and dielectric polarization is the same in these ferrites. A single ‘master curve’ for normalized plots of all the modulus isotherms observed for a given composition indicates that the distribution of relaxation time is temperature independent. The saturation magnetization and coercivity as calculated from the hysteresis loop measurement show striking dependence on composition.     

Interconversion of host–guest components in supramolecular assemblies of polycarboxylic acids and reduced Schiff bases

Eight supramolecular assemblies of benzene-1,3,5-tricarboxylic acid (H₃BTC) and benzene-1,2,4,5-tetracarboxylic acid (H₄BTtC) with reduced Schiff base of flexible backbone having phenolic and pyridyl groups, i.e., 1,2-bis(2-hydroxybenzylamino)ethane, 1,3-bis(2-hydroxybenzylamino)propane, 1,4-bis(2-hydroxybenzylamino)butane and 1,4-bis(4-pyridinylmethylamino)butane have been constructed by proton transfer reaction. H₃BTC forms host–guest type assemblies with amines having phenolic functionality, while a layered structure was obtained with pyridyl functionalized amine. H₄BTtC also formed host–guest assemblies with the diamines where reduced Schiff base acts as host and acid moiety acts as the guest. Different conformations of the diamines were observed in these assemblies. Theoretical studies were performed to analyze the effect of varied chain lengths of diamines on hydrogen bond interaction energy of the adducts.     

Partition functions and equilibrium constants of some positive molecular ions

Partition functions and equilibrium constants have been determined for the positively charged molecular ions CH⁺, NH⁺, OH⁺, MgH⁺, AlH⁺, SiH⁺, SH⁺, HCl⁺, CaH⁺, C⁺₂, CN⁺, CO⁺, N⁺₂, NO ⁺, SiO⁺ and for the molecule FeH.     

The status of trace and minor elements in some Bangladeshi foodstuffs

An investigation is conducted on the status of trace and minor elements in some foodstuffs (cereals, vegetables, milk, egg and fish), commonly consumed in Bangladesh, using proton induced X-ray emission (PIXE) and radioisotope-induced X-ray fluorescence (XRF) techniques. In PIXE measurements, the samples were irradiated in air with 2.0 MeV (energy on the target) protons having the beam intensity of 30 nA for characteristic X-ray excitation, while in XRF analysis, the samples were excited for 5000 seconds with a 10 mCi Cd-109 annular X-ray source. The elemental concentration of K, Ca, Mn, Fe, Ni, Cu, Zn, Se, As, Br, Rb, Sr, Mo, and Pb were determined in the samples by comparison with X-ray yield curves constructed from IAEA and NBS standard reference materials. The validity of the analytical procedures (PIXE and XRF) followed in this study has been confirmed by comparative measurements of Cu, Zn and Mn in some varieties of rice with atomic absorption spectrophotometry. The results indicate that none of the food regimes investigated here is burdened with heavy metals beyond permissible limits except five species of vegetables with chromium having the range of 0.99–3.59 mg/kg compared to the literature value of 0.0–0.36 mg/kg (dry weight basis). An average value of 0.2 mg/kg of arsenic was observed both in IRRI (n=16) and local Aman (n=12) varieties of rice and only one hen egg contained 1.7 mg/kg of lead in yolk. The zinc content in some marine fish from Bay of Bengal was reported to be 5.4–19.5 mg/kg, whereas in the present study of sweet-water fish, the level is found to be 15.2–62.1 mg/kg (fresh weight basis) for five species. In human milk, both Cu (0.12–0.25 mg/l, n=8) and Zn (0.28–1.80 mg/l, n=8) levels appear to be almost half the literature values (n=25). On the other hand formula milk has higher values of Cu (0.32–1.63 mg/kg, n=16) and Zn (5.16–19.8 mg/kg, n=16).     

Arsenic in drinking water and in scalp hair by EDXRF: A major recent health hazard in Bangladesh

Arsenic content in drinking water and in scalp hair of the arsenic affected areas in Bangladesh were measured using energy dispersive X-ray fluorescence (EDXRF) to determine the contribution of drinking water to body burden and health risks. Around 61% of the water analyzed from tube-wells has arsenic content above 0.05 mg/l and about 13% have arsenic content above 0.01 mg/l. The mean concentration of arsenic in contaminated water is about 0.26 mg/l with the maximum level of 0.83 mg/l. The contaminated water thus contributes a significant amount to the arsenic budget in humans in Bangladesh and consequently, to their health hazards. The average concentration of arsenic in hair of a patient group drinking contaminated water is 14.1 mg/kg where the normal levels are <3.0 mg/kg. The distribution of arsenic in water and in hair is compared and discussed with the data reported in the literature. The daily dietary intake value of arsenic by the adult population in Bangladesh is estimated and assessed signifying health effects.     

Graft copolymerization of 4-vinylpyridine onto cellulose using Co (III) acetylacetonate comlex in aqueous medium

The graft copolymerization of 4-vinylpyridine (4-VP) onto cellulose has been carried out in heterogeneous conditions with cobaltacetylacetonate complex (Co (acac)₃) under nitrogen atmosphere at 35±0.1°C in aqueous media. The grafting parameters such as graft yield, grafting efficiency, total conversion, frequency of grafting and rate of grafting have been evaluated as a function of concentration of 4-vinylpyridine, cobaltacetylacetonate and reaction temperature of graft copolymerization. Variation in concentration of monomer and initiator leads to a consistent increase in grafting parameters and then show a decreasing trend. The efficient grafting of monomer in presence of cobaltacetylacetonate complex is due to the coordination of the -electrons of the 4-vinylpyridine with the metal chelate which facilitate the homolytic decomposition of metal-oxygen bond to form radicals at relatively low temperature. The rate of graft copolymerization is directly proportional to the concentration of monomer and the square root of the concentration of the cobaltacetylacetonate complex. The activation energy (Ea) for graft copolymeriztion has been calculated using a Arrhenius plot and is 31.0kJ mol^–1 within the temperature range of 20–40°C. The grafting of 4-vinylpyridine has also been studied in presence of various additives and their effects have been suitably explained. On the basis of the experimental observations, reaction steps are proposed and rate expression has been derived.     

Intermediates in the reduction of the antituberculosis drug PA-824, (6S)-2-nitro-6-{[4-(trifluoromethoxy)benzyl]oxy}-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazine, in aqueous solution

The reduction chemistry of the new anti-tuberculosis drug PA-824, together with a more water-soluble analogue, have been investigated using pulse and steady-state radiolysis in aqueous solution. Stepwise reduction of these nitroimidazo-dihydrooxazine compounds through electron transfer from the CO(2) (-) species revealed that, unlike related nitroimidazoles, 2-electron addition resulted in the reduction of the imidazole ring in preference to the nitro group. In mildly acidic solution a nitrodihydroimidazo intermediate was formed, which was reduced further to the amine product. In both alkaline and neutral solution, an intermediate produced on 2-electron reduction was resistant to further reduction and reverted to parent compound on extraction or mass spectrometric analysis of the solution. The unusual reduction chemistry of these nitroimidazole compounds, exhibiting ring over nitro group reduction, is associated with alkoxy substitution in the 2-position of a 4-nitroimidazole. The unique properties of the intermediates formed on the reduction of PA-824 need to be considered as playing a possible role in its bactericidal action.