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11.
12.
Samir Mohamed El‐Moghazy Mohamed Abd El‐Azem Mohamed Marwa Fadel Mohamed Nadia Fayek Youssef 《中国化学会会志》2009,56(2):360-367
Reversed phase‐high performance liquid chromatography (RP‐HPLC), thin layer chromatography (TLC) densitometry and first derivative spectrophotometry (1D) techniques are developed and validated as a stability‐indicating assay of ezetimibe in the presence of alkaline induced degradation products. RP‐HPLC method involves an isocratic elution on a Phenomenex Luna 5μ C18 column using acetonitrile: water: glacial acetic acid (50:50:0.1 v/v/v) as a mobile phase at a flow rate of 1.5 mL/min. and a UV detector at 235 nm. TLC densitometric method is based on the difference in Rf‐values between the intact drug and its degradation products on aluminum‐packed silica gel 60 F254 TLC plates as stationary phase with isopropanol: ammonia 33% (9:1 v/v) as a developing mobile phase. On the fluorescent plates, the spots were located by fluorescence quenching and the densitometric analysis was carried out at 250 nm. Derivative spectrophotometry, the zero‐crossing method, ezetimibe was determined using first derivative at 261 nm in the presence of its degradation products. Calibration graphs of the three suggested methods are linear in the concentration ranges 1–10 mcg/mL, 0.1–1 mg/mL and 1–16 mcg/mL with a mean percentage accuracy of 99.05 ± 0.54%, 99.46 ± 0.63% and 99.24 ± 0.82% of bulk powder, respectively. The three proposed methods were successfully applied for the determination of ezetimibe in raw material and pharmaceutical dosage form; the results were statistically analyzed and compared with those obtained by the reported method. Validation parameters were determined for linearity, accuracy and precision; selectivity and robustness and were assessed by applying the standard addition technique. 相似文献
13.
Rasha A. M. Faty Hoda A. R. Hussein Ayman M. S. Youssef 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1484-1490
3-Ethyl 2-amino-4-methyl-5-phenyl thiophene carboxylate 1 was used as a starting material to synthesize 2a,b via coupling with malononitrile or acetyl acetone, respectively. When heated, under reflux in sodium ethoxide solution, 2a,b give 3a,b. On the other hand, when compounds 3a,b were heated under reflux in ethanol with hydrazine hydrate, thiourea, or 1,1-phenylenediamine hydrochloride and a catalytic amount of piperidine 4a,b, 5a,b and 6a,b, were produced, respectively. The new compounds were tested for their antimicrobial activity. Compounds 2a–6b showed antibacterial activities, and 2a,2b and 4b showed antifungal activities. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
14.
5-Amino-3-(3-methyl-5-oxo-1-phenyl-2-pyrazolin-4-yl)-7-phenyl-7H-thiazolo[3,2-a]pyrimidine-6-carbonitrile was synthesized via the reaction of 4-(2-aminothiazol-4-yl)-3-methyl-1-phenyl-2-pyrazolin-5-one with benzylidene malononitrile and was then transformed
to related fused heterocyclic systems. The antifungal and antibacterial studies revealed in some cases excellent biocidal
properties. 相似文献
15.
Tareq Youssef 《Photochemistry and photobiology》2009,85(4):921-926
Hypericin has been reported as a potent photosensitizing agent exhibiting antiviral, antibacterial, antineoplastic activities. Although its photophysics and mode of action are strongly modulated by the binding protein, detailed information about its mechanism of interaction with possible cellular targets, including proteins, is still lacking. Previous in vitro studies demonstrated that hypericin can be uptaken by intact lens and is able to bind to the major lens protein "α-crystallin." In this study, the mechanism of interaction of this potent drug with α-crystallin was studied using the chemical denaturant guanidine hydrochloride (GdnHCl) and the hydrophobic surface probe, 8-anilino-1-naphthalenesulfonic acid (ANS). Fluorescence measurements showed that the increased exposure of tryptophan resulting from partial unfolding of α-crystallin incubated with 1.0 mol L−1 of GdnHCl corresponds to the maximum accessibility of hydrophobic sites to ANS at the same GdnHCl concentration. Interestingly at this additional hydrophobicity of the protein, hypericin exhibited its maximum fluorescence intensity. This in vitro study implied that hydrophobic sites of α-crystallin play a significant role in its interaction with hypericin. The binding between α-crystallin and hypericin was found to be enhanced by partial perturbation of the protein. 相似文献
16.
Harrak Y Blaszykowski C Bernard M Cariou K Mainetti E Mouriès V Dhimane AL Fensterbank L Malacria M 《Journal of the American Chemical Society》2004,126(28):8656-8657
5-En-1-yn-3-ol substrates bearing a free hydroxyl group or an acyl group are highly versatile partners for PtCl2-catalyzed cycloisomerizations. Electrophilic activation of the alkyne moiety triggers at wish a hydride or an O-acyl migration yielding at the end to regioisomeric keto derivatives. The efficient preparation of Sabina ketone, an important monoterpene precursor, has been worked out. 相似文献
17.
Action of Hydrazines on 2‐(2‐Oxindolin‐3‐ylidene)malononitrile, (E,Z)‐Ethyl 2‐cyano‐2‐(2‐oxindolin‐3‐ylidene)acetate and Isatin‐β‐thiosemicarbazone as a Source of Spiro Indoline‐pyrazole Systems 下载免费PDF全文
Ahmed S. A. Youssef Magdy M. Hemdan Samir A. Emara Rabaa M. Kamel 《Journal of heterocyclic chemistry》2015,52(5):1331-1336
2‐(2‐Oxindolin‐3‐ylidene)malononitrile ( 1a ) or (E,Z)‐ethyl 2‐cyano‐2‐(2‐oxindolin‐3‐ylidene)acetate ( 1b ) or isatin‐β‐thiosemicarbazone ( 1c ) undergoes reactions with prototype hydrazine hydrate itself and some of its simple congeners to give hydrazone derivatives bearing indoline‐2‐one moiety ( 2 ). The hydrazone derivatives ( 2 ) when heated with acetyl acetone or ethyl acetoacetate in dry pyridine afforded the spiro indoline derivatives ( 3a , 3b ). Also, cinnoline derivative ( 9 ) is obtained by action of hydrazine hydrate on the N‐acetyl derivative of ( 6a ). The structures of the newly synthesized compounds were evaluated by IR, 1H‐NMR spectroscopy, mass spectra and elemental analyses. 相似文献
18.
Flood C Cosgrove T Qiu D Espidel Y Howell I Revell P 《Langmuir : the ACS journal of surfaces and colloids》2007,23(5):2408-2413
Solvent relaxation NMR and small-angle neutron scattering have been used to characterize adsorbed poly(ethylene oxide) (PEO) layers on silica at a range of surfactant and electrolyte concentrations. Below the critical aggregation concentration (cac), the results suggest that sodium dodecyl sulfate (SDS) interacts relatively weakly, perhaps analogously to a simple salt reducing the solvency of PEO. This is evidenced by a decrease in the adsorbed layer thickness combined with an increase in the bound fraction, although the total adsorbed amount is not greatly affected. The layer thickness goes through a minimum at the cac, after which further SDS addition results in the formation of PEO/SDS aggregates that repel each other and, hence, tend to desorb. The adsorbed amount therefore decreases, from 0.7 mg m(-2) initially to 0.2 mg m(-2) with 32 mM SDS. The aggregates that remain adsorbed also repel, and hence, there is an increase in the layer thickness and the persistence length, while the bound fraction is reduced. In comparison, the effects of electrolyte at the ionic strength studied are relatively minimal. There is, however, evidence that the repulsions between adsorbed PEO/SDS aggregates are partially screened, allowing them to approach each other more readily. This leads to a contraction of the adsorbed layer when the SDS concentration is sufficiently high. 相似文献
19.
Habibi Y Foulon L Aguié-Béghin V Molinari M Douillard R 《Journal of colloid and interface science》2007,316(2):388-397
The goal of this work is the preparation of monolayers of cellulose I nanocrystals providing flat crystalline cellulose surfaces. Suspensions of cellulose nanocrystals were prepared by hydrolyzing ramie and tunicin fibers with sulfuric acid. Due to surface grafted sulfate groups, the negatively charged, rod-like cellulose nanocrystals were found to form stable layers at the air-water interface in the presence of a cationic amphiphilic molecule such as dioctadecyldimethylammonium (DODA) used in this work. These layers were formed at different cellulose-DODA weight ratios, compressed and analyzed by tensiometry, ellipsometry and Brewster angle microscopy. At low cellulose concentrations the layers are discontinuous, becoming dense and homogeneous upon reaching a critical weight ratio, which depends on the aspect ratio of the cellulose nanocrystals. After transfer onto silicon wafers, the surface composition and morphology as well as the thickness of the films were examined by X-ray photoelectron spectroscopy, ellipsometry and atomic force microscopy. The results indicate that they are monolayer films, well structured, relatively smooth and pure. These films offer a crystalline and easily reproducible model cellulose surface. 相似文献
20.
The effects of a ready-made surfactant (sodium dodecyl sulfate) on the dynamic interfacial tension between a model acidic oil (linoleic acid dissolved in paraffin oil) and various aqueous alkaline (NaOH) systems have been studied using pendant drop tensiometry at surfactant concentrations both below and above the critical micelle concentration (CMC). Below the CMC the added surfactant contributes significantly to a further reduction of interfacial tension of the reacting acid/alkaline system, whereas above the CMC the added surfactant plays an important role in damping the dynamic trends observed for the reactive system alone. Copyright 2001 Academic Press. 相似文献