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A novel family of chelating bis-bidentate azodye compounds1 with Cu(II), Co(II), Ni(II), Fe(II), Hg(II), Pd(II), UO2(II), Fe(III), Cr(III), La(III), Ru(III) and Zr(IV) has been prepared and characterized on the basis of analytical, magnetic, 1H and 13C NMR, EPR and electronic spectral studies. Tentative structures for the polymeric complexes are proposed. The important IR bands and the main 1H and 13C signals are assigned and discussed relative to the molecular structure. Various EPR parameters for Cμ(II), have been calculated. The ligand acts as a dibasic bis-bidentate chelating agent coordinating through CO, N=N, COOH and OH groups by replacement of a proton from the two latter groups. Considerable interest has also been focused on the synthesis of the azo compound and its polymeric metal complex due to its wide potential applications. The thermal decomposition behavior of the complexes is also discussed. 相似文献
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Nageswara Rao R Mastan Vali R Vara Prasada Rao A 《Journal of separation science》2012,35(15):1945-1952
An efficient and environmental friendly ionic liquid based dispersive liquid-liquid microextraction procedure was optimized for determination of rifaximin in rat serum by reverse phase high-performance liquid chromatography. The effect of ionic liquids, dispersive solvents, extractant/disperser ratio, and salt concentrations on sample recovery and enrichment factors were studied. Among the five ionic liquids studied in the present investigation, 1-butyl-3-methylimidazolium hexafluorophosphate was found to be most effective for extraction of rifaximin. The recovery was found to be more than 98% using 1-butyl-3-methylimidazolium hexafluorophosphate and methanol as extraction and dispersive solvents, at an extractant/disperser ratio of 0.43. The recovery was further enhanced to 99.5% by the addition of 5.0% NaCl solution. A threefold enhancement in detection limit was achieved when compared to protein precipitation. The ionic liquid containing the extracted rifaximin was directly injected into HPLC system. The linear relationship was observed in the range of 0.03-10.0 μg/mL with the correlation coefficient (r(2) ) 0.9998. Limits of detection and quantification were found to be 0.01 and 0.03 μg/mL, respectively. The relative standard deviation was 2.5%. The method was validated and applied to study pharmacokinetics of rifaxmin in rat serum. 相似文献
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