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Agüera A Pérez Estrada LA Ferrer I Thurman EM Malato S Fernández-Alba AR 《Journal of mass spectrometry : JMS》2005,40(7):908-915
Exact mass capabilities of time-of-flight (TOF) mass spectrometry along with other mass spectrometric techniques have been evaluated to elucidate a complete range of dichlofenac phototransformation products. Photolysis experiments with diclofenac in water under direct solar irradiation were performed to characterise the main phototransformation products generated and to determine their stability. Photolysis experiments were performed in both demineralised water and reconstructed standard freshwater. Samples were extracted before analysis by solid phase extraction (SPE) with Oasis HLB and MAX cartridges. Separation and identification of the transformation products were accomplished by the combined use of gas chromatography-mass spectrometry (GC/MS) and liquid chromatography coupled with time-of-flight mass spectrometry (LC/TOFMS). Both techniques provided complementary information that enabled the identification of 13 phototransformation products. Six of them were identified by GC/MS through the structural information provided by the full scan mass spectra obtained under electron impact (EI) ionisation and the confirmation of the molecular mass provided by positive chemical ionisation (PCI) analyses. Accurate mass measurements obtained by LC/TOFMS provided the elucidation of seven polar transformation products. The low mass error observed (<2 ppm) enabled the assignment of highly probable empirical formulas as well as identification of a process dimerisation route. The photoproducts identified demonstrated that photolysis of diclofenac occurs by two main routes. One is the consequence of the initial photocyclisation of diclofenac into carbazole derivatives. The other route goes through the initial decarboxilation of diclofenac and further oxidation of the alkyl-chain, which are typical photolytic process reactions. The main photoproduct identified was 8-chloro-9H-carbazole-1yl-acetic acid. 相似文献
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Apirat Laobuthee Hatsuo Ishida Suwabun Chirachanchai 《Journal of inclusion phenomena and macrocyclic chemistry》2003,46(3-4):179-185
This study was carried out with the aim to optimize the dissolution propertiesof diclofenac (DIC) – a non-steroidal anti-inflammatory drug sparingly solublein water – through association -with -cyclodextrin (CD). Theeffect of CD on the aqueous solubility of DIC was evaluated by thephase solubility method. The amount of DIC dissolved increased linearly withthe addition of CD according to an AL type plot and without precipitationof the complex. The apparent stability constant of the complex, calculated supposinga 1:1 stoichiometry, was 295 M-1; this value was confirmed by circulardichroism analysis. DIC/CD interactions were also studied in water by1H and 13C NMR spectroscopy. Equimolar DIC/CD solid systems were prepared by physical-mixing, kneading, co-evaporation andfreeze-drying, and their properties in the solid state studied by DifferentialScanning Calorimetry, X-ray powder diffractometry and Fourier-TransformInfrared analysis. For sake of comparison, the mixture of DIC and CDseparately lyophilized was investigated too. The results demonstrated that thefreeze-dried product had the highest degree of amorphization and they were inagreement with the existence of an inclusion complex in the solid state. Thedissolution profiles of the drug from each solid system were affected by its physico-chemical properties, the freeze-dried being the most rapidly dissolvingforms. 相似文献
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Sevim Hamamci Alisir Necmi Dege Recep Tapramaz 《Acta Crystallographica. Section C, Structural Chemistry》2019,75(4):388-397
Three new diclofenac‐based copper(II) complexes, namely tetrakis{μ‐2‐[2‐(2,6‐dichloroanilino)phenyl]acetato‐κ2O:O′}bis(methanol‐κO)copper(II), [Cu2(μ‐dicl)4(CH3OH)2] ( 1 ), bis{2‐[2‐(2,6‐dichloroanilino)phenyl]acetato‐κ2O,O′}bis(1‐vinyl‐1H‐imidazole‐κN3)copper(II), [Cu(dicl)2(vim)2] ( 2 ), and bis{2‐[2‐(2,6‐dichloroanilino)phenyl]acetato‐κ2O,O′}bis(1H‐imidazole‐κN3)copper(II), [Cu(dicl)2(im)2] ( 3 ) [dicl is diclofenac (C14H10Cl2NO2), vim is 1‐vinylimidazole (C5H6N2) and im is imidazole (C3H4N2)], have been synthesized and characterized by elemental analysis, FT–IR spectroscopy, thermal analysis and single‐crystal X‐ray diffraction. X‐ray diffraction analysis shows that complex 1 consists of dimeric units in which the dicl ligand exhibits a bidentate syn,syn‐μ2 coordination mode linking two copper(II) centres. Complexes 2 and 3 have mononuclear units with the general formula [Cu(dicl)2L2] (L is vim or im) in which the CuII ions are octahedrally coordinated by two L and two dicl chelating ligands. The L and dicl ligands both occupy the trans positions of the coordination octahedron. The different coordination modes of dicl in the title complexes were revealed by Fourier transform IR (FT–IR) spectroscopy. The spin matching between the copper(II) centres in the dimeric [Cu2(μ‐dicl)4(CH3OH)2] units was also confirmed by magnetic data to be lower than the spin‐only value and electron paramagnetic resonance (EPR) spectra. The thermal properties of the complexes were investigated by thermogravimetric (TG) and differential thermal analysis (DTA) techniques. 相似文献
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Marcelo Kobelnik Douglas Lopes Cassimiro Diógenesdos Dos Santos Clóvis Augusto Ribeiro Marisa Spirandeli Crespi 《中国化学》2011,29(11):2271-2277
Solid state compounds of general formula Sr(Diclof)2·5.7H2O and Ba(Diclof)2·4.8H2O were obtained. Thermogravimetry (TG), differential scanning calorimetry (DSC), X‐ray diffraction powder patterns and microscopy analysis were used to characterize these compounds. Details concerning the dehydration and thermal decomposition as well as data of kinetic parameters have been described here. The kinetic behaviors of these stages were evaluated from several heating rates with samples masses of 2 and 5 mg in open crucibles under a nitrogen atmosphere. The results of the present study improve the knowledge on these compounds including their dehydration and thermal stability. The obtained data depend on the mass of the sample which results in two kinetic behavior patterns. 相似文献
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Mario Suwalsky Marcela Manrique Fernando Villena Carlos P. Sotomayor 《Macromolecular Symposia》2010,296(1):436-445
Phospholipids are amphipatic molecules with long hydrophobic acyl chains and zwitterionic polar heads which assemble into different types of molecular aggregates. The most relevant is the bilayer because of its relation with cell membranes, which are very complex entities. For this reason, simpler molecular models based on phospholipids bilayers are widely used. We have determined the bilayer structure of phospholipids located in the outer and inner monolayers of most cell membranes, and use them as molecular models to study the way different chemicals of biological interest interact with cell membranes. We present the results of our studies on the nonsteroidal anti-inflammatory drug diclofenac, from which little is known about its effects on human erythrocytes. This report presents the following evidence that diclofenac interacts with the human red cell membrane: a) X-ray diffraction and fluorescence spectroscopy of phospholipids bilayers show that diclofenac interacts with a class of lipids found in the outer moiety of the erythrocyte membrane; b) in isolated unsealed human erythrocyte membranes the drug induced a disordering effect on the acyl chains of the membrane lipid bilayer; c) in scanning electron microscopy studies on human erythrocytes it was observed that the drug induced morphological changes different from their normal biconcave shape. 相似文献
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《Journal of separation science》2018,41(7):1644-1650
A novel, simple, and inexpensive analytical technique based on flat sheet supported liquid membrane microextraction coupled with fast Fourier transform stripping cyclic voltammetry on a reduced graphene oxide carbon paste electrode was used for the extraction and online determination of diclofenac in whole blood. First, diclofenac was extracted from blood samples using a polytetrafluoroethylene membrane impregnated with 1‐octanol and then into an acceptor solution, subsequently it was oxidized on a carbon paste electrode modified with reduced graphene oxide nanosheets. The optimal values of the key parameters influencing the method were as follows: scan rate, 6 V/s; stripping potential, 200 mV; stripping time, 5 s; pH of the sample solution, 5; pH of the acceptor solution,7; and extraction time, 240 min. The calibration curves were plotted for the whole blood samples and the method was found to have a good linearity within the range of 1–25 μg/mL with a determination coefficient of 0.99. The limits of detection and quantification were 0.1 and 1.0 μg/mL, respectively. Using this coupled method, the extraction and determination were merged into one step. Accordingly, the speed of detection for sensitive determination of diclofenac in complex samples, such as blood, increased considerably. 相似文献
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Sevim Hamamci Alisir Necmi Dege 《Acta Crystallographica. Section C, Structural Chemistry》2016,72(12):947-951
AgI‐containing coordination complexes have attracted attention because of their photoluminescence properties and antimicrobial activities and, in principle, these properties depend on the nature of the structural topologies. A novel two‐dimensional silver(I) complex with the anti‐inflammatory diclofenac molecule, namely bis{μ‐2‐[2‐(2,6‐dichloroanilino)phenyl]acetato‐κ3O,O′:O}bis(μ‐2,5‐dimethylpyrazine‐κ2N:N′)silver(I), [Ag2(C14H10Cl2NO2)2(C6H8N2)]n, (I), has been synthesized and characterized by single‐crystal X‐ray diffraction, revealing that the AgI ions are chelated by the carboxylate groups of the anionic 2‐[2‐(2,6‐dichloroanilino)phenyl]acetate (dicl) ligand in a μ3‐η1:η2 coordination mode. Each dicl ligand links three AgI atoms to generate a one‐dimensional infinite chain. Adjacent chains are connected through 2,5‐dimethylpyrazine (dmpyz) ligands to form a two‐dimensional layer structure parallel to the crystallographic bc plane. The layers are further connected by C—H…π interactions to generate a three‐dimensional supramolecular structure. Additionally, the most striking feature is that the structure contains an intramolecular C—H …Ag anagostic interaction. Furthermore, the title complex has been tested for its in vitro antibacterial activity and is determined to be highly effective on the studied microorganisms. 相似文献
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Ahmed H. Ragab Hala S. Hussein Inas A. Ahmed Khamael M. Abualnaja Najla AlMasoud 《Molecules (Basel, Switzerland)》2021,26(17)
Based on the adsorption performance of a porous nanocomposite with limestone (LS), activated carbon (AC) and sodium alginate (SG), a unique, multifunctional LS–AC–SG nanocomposite absorbent was designed and prepared for extracting antibiotics and drugs from aqueous solutions. The composite exhibited the following advantages: quick and simple to prepare, multifunctionality and high efficiency. Amoxicillin (AMX) and diclofenac (DCF) were chosen as the conventional antibiotic and the drug, respectively. The prepared nanocomposite’s physicochemical characteristics were calculated through numerous characterization methods. The structure of the surface was made up of interconnected pores that can easily confine pollutants. The surface area was measured to be 27.85 m2/g through BET analysis. The results show that the maximum absorption capacity of amoxicillin and diclofenac was 99.6% and 98.4%, respectively, at a contact time of 40 min. The maximum removal of amoxicillin and diclofenac was reached at pH = 2. Adsorption analysis revealed that adsorption isotherm and kinetic data matched the pseudo-first-order kinetic and the Langmuir isotherm models. The results imply that the synthesized nanocomposites have the capacity to remove amoxicillin (AMX) and diclofenac (DCF) from aqueous solutions. 相似文献