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51.
Three reliable, rapid and selective methods have been developed and validated for the determination of lamotrigine in the presence of its impurity, 2,3-dichlorobenzoic acid. The first method is spectrophotometric method using p-chloranilic acid forming a colored product with lambda(max) 519+/-2 nm. All variables affecting the reaction have been investigated and the conditions were optimized. Beer's law was obeyed over a concentration range of 10-200 microg ml(-1) with mean accuracy 100.13+/-0.44%. The molar ratio of the formed ion-association complex is found to be 1 : 1 as deduced by Job's method. The conditional stability constant (K(f)), standard free energy (DeltaG), molar absorptivity(epsilon), and sensitivity index were evaluated. The second method is based on TLC separation of the cited drug (Rf=0.75+/-0.01) from its impurity (Rf=0.23+/-0.01) followed by densitometric measurement of the intact drug spots at 275 nm. The separation was carried on silica gel plates using ethyl acetate : methanol : ammonia 35% (17 : 2 : 1 v/v/v) as a mobile phase. The linearity range was 0.5-10 microg/spot with mean accuracy 99.99+/-1.33%. The third method is accurate and sensitive stability-indicating HPLC method based on separation of lamotrigine from its impurity on a reversed phase C(18) column, using a mobile phase of acetonitrile : methanol : 0.01 M potassium orthophosphate (pH 6.7+/-0.1) (30 : 20 : 50 v/v/v) at ambient temperature 25+/-5 degrees C and UV detection at 275 nm in an overall analysis time of about 6 min., based on peak area. The injection repeatability, intraday and interday repeatability were calculated. The procedure provided a linear response over the concentration range 1-12 microg ml(-1) with mean accuracy of 99.50+/-1.30%. The proposed methods were successfully applied for the determination of lamotrigine in bulk powder, in dosage form and in presence of its impurity. The results obtained were analyzed by ANOVA to assess that no significant difference between each of the three methods and the reported one. The validation was performed according to USP guidelines. 相似文献
52.
Behery FA Naeem ZE Maatooq GT Amer MM Wen ZH Sheu JH Ahmed AF 《Chemical & pharmaceutical bulletin》2007,55(8):1264-1266
The novel natural product juncutol (1), 1,4,7-trimethyl-8,9-dihydro-4H-cyclopenta[def]phenanthrene-2,6-diol, along with the three related metabolites juncusol (2), dehydrojuncusol (3), and 6-hydroxymethyl-1-methyl-5-vinyl-9,10-dihydrophenanthrene-2-ol (4), were isolated from the rhizomes of Juncus acutus L. (Juncaceae) growing in Egypt. The structural identity of 1 was determined on the basis of spectroscopic analyses, including 2D NMR spectroscopy. The inhibitory effect of these natural products on the expression of inducible nitric oxide synthase (iNOS) in lipopolysaccharide-stimulated RAW264.7 macrophage cells was determined for the first time. The unprecedented symmetrical compound juncutol (1) was found to be the most potent inhibitor against the induction of the proinflammatory iNOS protein. 相似文献
53.
Waqas Jamil Sorath Solangi Muhammad Ali Khalid Muhammad Khan Muhammad Taha Muhammad Yar Khuhawar 《Arabian Journal of Chemistry》2019,12(8):2262-2269
2-Hydroxy salicylhydrazide isatin hydrazone (L) and its Mn (II), Co (II), Ni (II), Cu (II), and Zn (II), metal complexes were synthesized. 1H NMR, UV–Vis, IR spectroscopy and elemental (CHN/S) analysis techniques were applied for characterization. TG/DTA techniques revealed that all the synthetic compounds are thermally stable up to 300 °C. They were found non-electrolytes in nature. Furthermore, all these complexes were evaluated for antiglycation and DPPH radical scavenging activities. They showed varying degree of activity with IC50 values between 168.23 and 269.0 μM in antiglycation and 29.63–57.71 μM in DPPH radical scavenging activity. Mn (II), Co (II), Ni (II), Cu (II), and Zn (II), metal complexes showed good antiglycation as well as DPPH radical scavenging activity. The IC50 values for antiglycation activity are 168.23 ± 2.37, 234.27 ± 4.33, 257.1 ± 6.43, 267.7 ± 8.43, 269.0 ± 8.56 Ni for Co, Zn, Mn, Cu, and Ni complexes, respectively, while IC50 value were found to be 29.63 ± 2.76, 31.13 ± 1.41, 35.16 ± 2.45, 43.53 ± 3.12, 57.71 ± 2.61 μM for Cu, Zn, Mn, Co and Ni complexes, respectively, for DPPH radical scavenging activity. These synthesized metal complexes were found to be better active than standards Rutin (IC50 = 294.46 μM) for anti-glycation, and tert-butyl-4-hydroxyanisole (IC50 = 44.7 μM) for DPPH radical scavenging activity. 相似文献
54.
A. K. Arof N. A. Mat Nor N. R. Ramli N. Aziz I. M. Noor R. M. Taha 《Optical and Quantum Electronics》2017,49(1):37
Photoelectrodes of dye-sensitized solar cells (DSSCs) have been prepared using nanosized titanium dioxide that have soaked in a solution of different saffron (Crocus sativus L.) spice content in ethanol. The optimized polyacrylonitrile (PAN)-based gel polymer electrolyte with 40.93 wt.% ethylene carbonate, 37.97 wt.% propylene carbonate, 4.37 wt.% tetrapropylammonium iodide, 9.86 wt.% PAN, 1.24 wt.% 1-butyl-3-methylimidazolium iodide, 4.35 wt.% lithium iodide and 1.28 wt.% iodine has been used as the electrolyte for DSSC. The electrolyte has conductivity of 2.91 mS cm?1 at room temperature (298 K). DSSCs were also sensitized with saffron solution that has been added with 30 wt.% chenodeoxycholic acid (CDCA) co-adsorbent and designated as DSSC P4. The solar cell converts light-to-electricity at an efficiency of 0.31%. This is 29% enhancement in efficiency for the DSSC without addition of CDCA in the saffron-ethanol solution. The DSSC exhibits current density at short-circuit (J sc ) of 1.26 mA cm?2, voltage at open circuit (V oc ) of 0.48 V and 51% fill factor. DSSC P4 also exhibits the highest incident photon-to-current density of more than 40% at 340 nm wavelength. 相似文献
55.
Biological buffers are of utmost importance for research in biological and clinical chemistry and in oceanography, but they may not be inert enough, thus interfering with the system under study. The N-[Tris(hydroxymethyl)methyl]-3-aminopropanesulfonic acid (TAPS) and N-[Tris(hydroxymethyl)methyl]-3-amino-2-hydroxypropanesulfonic acid (TAPSO) are useful zwitterionic buffers for pH control as standard buffers in the physiological region of pH 7.7 to 9.1 for TAPS and 7.0 to 8.2 for TAPSO, respectively. In this work, interaction between these zwitterionic compounds and electrolytes of potassium acetate (KAc), potassium bromide (KBr), potassium chloride (KCl), and sodium chloride (NaCl) were investigated through measuring the densities of these buffers in aqueous and in aqueous electrolyte solutions by a high precision vibrating tube digital densitometer from T = (298.15 to 328.15) K under atmospheric pressure. In this series of measurements, the aqueous samples were prepared with various concentrations of the zwitterionic buffers, up to saturated conditions, and over salt concentrations from (1 to 4) mol · dm?3. The measured densities served to evaluate the cubic expansion coefficients, α(m, T) and the apparent molar volumes, V?(m, T). An empirical equation was used to correlate quantitatively the experimental densities over the entire concentration ranges. 相似文献
56.
Ya‐Ching Shen Pei‐Show Shih Yun‐Sheng Lin Yu‐Chi Lin Yao‐Haur Kuo Yuh‐Chi Kuo Ashraf Taha Khalil 《Helvetica chimica acta》2009,92(10):2101-2110
Chemical investigation of the sponge Ircinia formosana resulted in the isolation of seven new linear C22‐sesterterpenoids, irciformonins E–K ( 1 – 7 ) in addition to irciformonin A ( 8 ), a previously isolated furanosesterterpenoid (=a furan‐moiety‐containing sesterterpenoid) from the same species. The structures were determined by interpretation of HR‐ESI‐MS and 2D‐NMR spectra. The structure of irciformonin A ( 8 ) was revised. Compound 5 exhibited significant inhibition of peripheral blood mononuclear cell proliferation induced by phytohemaglutinin. 相似文献
57.
Rezai T Yu B Millhauser GL Jacobson MP Lokey RS 《Journal of the American Chemical Society》2006,128(8):2510-2511
Little is known about the effect of conformation on passive membrane diffusion rates in small molecules. Evidence suggests that intramolecular hydrogen bonding may play a role by reducing the energetic cost of desolvating hydrogen bond donors, especially amide N-H groups. We set out to test this hypothesis by investigating the passive membrane diffusion characteristics of a series of cyclic peptide diastereomers based on the sequence cyclo[Leu-Leu-Leu-Leu-Pro-Tyr]. We identified two cyclic hexapeptide diastereomers based on this sequence, whose membrane diffusion rates differed by nearly two log units. Results of solution NMR studies and hydrogen/deuterium (H/D) exchange experiments showed that membrane diffusion rates correlated with the degree of intramolecular hydrogen bonding and H/D exchange rates. The most permeable diastereomer, cyclo[d-Leu-d-Leu-Leu-d-Leu-Pro-Tyr] (1), exhibited a passive membrane diffusion rate comparable to that of the orally available drug cyclosporine A. 相似文献
58.
59.
A.S. Shalabi A.M. El Mahdy M.M. Assem H.O. Taha W.S. Abdel Halim 《Molecular physics》2014,112(1):22-34
Molecular electronic structure calculations, employing density functional theory (DFT) and time-dependent density functional theory (TD-DFT) methodologies, have been carried out to improve the performance of the synthesised dye YD2-o-C8 which is characterised by 11.9%–12.7% efficiencies. We aimed to narrow the band gap of YD2-o-C8 to extend the light-harvesting region to near-infrared (NIR). This was done by incorporating Cd instead of Zn onto the porphyrin ring and elongating the length of π-conjugation by adding ethynylene link and anthracene unit, so that the performances of the suggested cells could be expected to exceed the 11.9%–12.7% efficiencies with TiO2, ZnO2, and WO3 oxide electrodes. The effects of modifying the central metal and elongating the length of π-conjugation on cell performance are confirmed in terms of frontier molecular orbital (FMO) energy gaps, density of states (DOS), molecular electrostatic potentials (MEPs), non-linear optical (NLO) properties, ultraviolet–visible (UV–vis) electronic absorption, and 1H nuclear magnetic resonance chemical shifts. Increasing the length of π-conjugation of the D–π–A dyes leads to increasing the DOS near Fermi levels, more active NLO performance, strong response to the external electric field, delocalisation of the negative charges near the anchoring groups, deep electron injection, suppressing macrocycle aggregation, active dye regeneration, and inhibited dye recombination. The calculated band gap/eV of the present DMP-Zn is correlated with the experimental (E1/2(oxidation)–E1/2(reduction)/V) potentials of the identical YD2-o-C8. A co-sensitiser is suggested for NIR sensitisation (550–950 nm) to increase the power-to-conversion efficiency beyond 14%. 相似文献
60.
M. Hafez I. S. Yahia S. Taha 《Applied Physics A: Materials Science & Processing》2014,116(3):1445-1453
Optical, microstructural, and thermal properties of the investigated silver nitrate samples were characterized by various techniques, such as X-ray analysis, scanning electron microscopy, UV–Vis–NIR absorption and differential scanning calorimetry (DSC). The presence of structural phase transition [orthorhombic structure (phase II) to rhombohedral structure (phase I)] was checked by DSC and X-ray analysis measurements. The thermal energy required for such transformation is found to be 11.6 J/g. The optical band gaps of AgNO3 are 1.4 and 2.02 eV for phase II and phase I, respectively, at the low-energy region. But at high-energy region, the optical band gaps are 3.41 and 3.43 eV for phase II and phase I, respectively. Characteristic peaks for AgNO3 corresponding to (2 1 1), (0 0 4) and (3 5 1) for phase II and (0 0 4), (3 1 1) and (0 2 4) for phase I have been observed. The average crystalline size for AgNO3 samples and the values of dislocation density δ and the strain ε for the planes of two phases II and I are calculated and also the texture coefficient is determined. Such information can considerably aid in understanding the process of phase transformations in AgNO3. 相似文献