Two new complexes [Pd（L-phe）2·2H2O] （1） and [Pd（4,4＇-dcbpy）（en）·H2O] （2） （L-phe = L-phenylalanine, 4,4＇-dcbpy = 2,2＇-bipyridyl-4,4＇-dicarboxylate, en = ethylenediamine） were synthesized and c...Two new complexes [Pd（L-phe）2·2H2O] （1） and [Pd（4,4＇-dcbpy）（en）·H2O] （2） （L-phe = L-phenylalanine, 4,4＇-dcbpy = 2,2＇-bipyridyl-4,4＇-dicarboxylate, en = ethylenediamine） were synthesized and characterized. L-phenylalanine was in situ formed via the hydrolysis of N-（tert-butoxycarbonyl）-L-phenylalanine, and ethylenediamine came from the in situ reaction of piperazine （pip） under hydrothermal conditions. The single-crystal X-ray structure analyses reveal that the Pd（Ⅱ） ion constructs a square planer coordination geometry in complexes 1 and 2, respectively. Complex 1 extends into a 2D layered structure via H-bond interactions and complex 2 connects into a 3D network through hydrogen bonds and 7r-tr stacking interactions. The interactions of 1 and 2 with fish sperm DNA （FS-DNA） were examined via UV-Vis absorption spectra and fluorescence spectroscopy. The cleavage reaction for plasmid DNA has been assayed by agarose gel electrophoresis. The results indicate that two complexes interact with DNA and the insertion is the main binding mode.展开更多
An optimized and validated spectrophotometric method has been developed for the determination of cefixime in pharmaceutical formulations. The method is based on the complexa- tion reaction between cefixime and palladi...An optimized and validated spectrophotometric method has been developed for the determination of cefixime in pharmaceutical formulations. The method is based on the complexa- tion reaction between cefixime and palladium ion in the presence of acidic buffer solution （pH 3） in ethanol-distilled water medium at room temperature. The complex absorbed maximally at 352 nm. Beer＇s law is obeyed in the working concentration range of 2.5-35 μg/mL with apparent molar absorptivity of 1.015×104 L/mol cm and Sandell＇s sensitivity of 0.001 μg/cm2/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.175 and 0.583μg/mL, respectively. The effect of common excipients used as additives has been studied in the determination of cefixime. The proposed method has been successfully applied for the determina- tion of cefixime in pharmaceutical formulations. The results obtained by the proposed method were statistically compared with the reference method using t and F values and found no significant difference between the two methods.展开更多
基金conducted in the framework of a project sponsored by the National Natural Science Foundation of China(No.21071100)Program for Liaoning Excellent Talents in University(LJQ2014043)
文摘Two new complexes [Pd（L-phe）2·2H2O] （1） and [Pd（4,4＇-dcbpy）（en）·H2O] （2） （L-phe = L-phenylalanine, 4,4＇-dcbpy = 2,2＇-bipyridyl-4,4＇-dicarboxylate, en = ethylenediamine） were synthesized and characterized. L-phenylalanine was in situ formed via the hydrolysis of N-（tert-butoxycarbonyl）-L-phenylalanine, and ethylenediamine came from the in situ reaction of piperazine （pip） under hydrothermal conditions. The single-crystal X-ray structure analyses reveal that the Pd（Ⅱ） ion constructs a square planer coordination geometry in complexes 1 and 2, respectively. Complex 1 extends into a 2D layered structure via H-bond interactions and complex 2 connects into a 3D network through hydrogen bonds and 7r-tr stacking interactions. The interactions of 1 and 2 with fish sperm DNA （FS-DNA） were examined via UV-Vis absorption spectra and fluorescence spectroscopy. The cleavage reaction for plasmid DNA has been assayed by agarose gel electrophoresis. The results indicate that two complexes interact with DNA and the insertion is the main binding mode.
文摘An optimized and validated spectrophotometric method has been developed for the determination of cefixime in pharmaceutical formulations. The method is based on the complexa- tion reaction between cefixime and palladium ion in the presence of acidic buffer solution （pH 3） in ethanol-distilled water medium at room temperature. The complex absorbed maximally at 352 nm. Beer＇s law is obeyed in the working concentration range of 2.5-35 μg/mL with apparent molar absorptivity of 1.015×104 L/mol cm and Sandell＇s sensitivity of 0.001 μg/cm2/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.175 and 0.583μg/mL, respectively. The effect of common excipients used as additives has been studied in the determination of cefixime. The proposed method has been successfully applied for the determina- tion of cefixime in pharmaceutical formulations. The results obtained by the proposed method were statistically compared with the reference method using t and F values and found no significant difference between the two methods.
