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Excellent Separation (excellent + separation)
Selected AbstractsSilver Amalgam Film Electrode of Prolonged Application in Stripping ChronopotentiometryELECTROANALYSIS, Issue 18 2007Kapturski Abstract The utility of the cylindrical silver-based mercury film electrode of prolonged analytical application in stripping chronopotentiometry (SCP) was examined. This electrode allowed us to obtain good reproducibility of results owing to the special electrode design, which enables regeneration of the thin layer before each measurement cycle. The accessible potential window in KNO3 (pH,2), acetate and ammonia buffers was defined, and the optimal conditions (i.e., stripping current, deposition potential and deposition time) for the determination of Cd and Pb traces were selected. The detection limits, obtained for an accumulation time of 60,s, were 0.023,,g/L for Cd and 0.075,,g/L for Pb. The response increases linearly with Cd, Pb and Zn concentration, up to at least 100,,g/L. It was also shown that the proposed procedure ensures excellent separation of the In and Tl, Pb and Tl or the In and Cd signals. The method was tested with dolomite and lake sediment samples, and good agreement with reference values was achieved. The obtained results showed good reproducibility (RSD=5,6%) and reliability. [source] Preparation and characterization of a molecularly imprinted monolithic column for pressure-assisted CEC separation of nitroimidazole drugsELECTROPHORESIS, Issue 16 2010Sulan Liao Abstract A polymethacrylate-based molecularly imprinted monolithic column bearing mixed functional monomers, using non-covalent imprinting approach, was designed for the rapid separation of nitroimidazole compounds. The new monolithic column has been prepared via simple in situ polymerization of 2-hydroxyethyl methacrylate, dimethylaminoethyl methacrylate and ethylene dimethacrylate, using (S)-ornidazole ((S)-ONZ) as template in a binary porogenic mixture consisting of toluene and dodecanol. The composition of the polymerization mixture was systematically altered and optimized by altering the amount of monomers as well as the composition of the porogenic solvent. The column performance was evaluated in pressure-assisted CEC mode. Separation conditions such as pH, voltage, amount of organic modifier and salt concentration were studied. The optimized monolithic column resulted in excellent separation of a group of structurally related nitroimidazole drugs within 10,min in isocratic elution condition. Column efficiencies of 99,000, 80,000, 103,000, 60,000 and 99,000,plates/m were obtained for metronidazole, secnidazole, ronidazole, tinidazole and dimetridazole, respectively. Parallel experiments were carried out using molecularly imprinted and non-imprinted capillary columns. The separation might be the result of combined effects including hydrophobic, hydrogen bonding and the imprinting cavities on the (S)-ONZ-imprinted monolithic column. [source] A fully automated 2-D LC-MS method utilizing online continuous pH and RP gradients for global proteome analysisELECTROPHORESIS, Issue 23 2007Hu Zhou Abstract The conventional 2-D LC-MS/MS setup for global proteome analysis was based on online and offline salt gradients (step and continuous) using strong-cation-exchange chromatography in conjunction with RP chromatography and MS. The use of the online system with step salt elution had the possibility of resulting in peptide overlapping across fractions. The offline mode had the option to operate with continuous salt gradient to decrease peak overlap, but exhibited decreased robustness, lower reproducibility, and sample loss during the process. Due to the extensive washing requirement between the chromatography steps, online continuous gradient was not an option for salt elution. In this report, a fully automated, online, and continuous gradient (pH continuous online gradient, pCOG) 2-D LC-MS/MS system is introduced that provided excellent separation and identification power. The pH gradient-based elution provided more basic peptides than that of salt-based elution. Fraction overlap was significantly minimized by combining pH and continuous gradient elutions. This latter approach also increased sequence coverage and the concomitant confidence level in protein identification. The salt and pH elution-based 2-D LC-MS/MS approaches were compared by analyzing the mouse liver proteome. [source] Separation of structural, geometrical and optical isomers of epoxycarotenoids using triacontyl-bonded stationary phasesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 11 2009Antonio J. Meléndez-Martínez Abstract The efficiency of C30 stationary phases in the separation of carotenes and diverse hydroxycarotenoids has been the subject of several studies. However, little is known concerning their ability to resolve epoxycarotenoids isomers, whose study is of great importance due to the functions they serve and the information they can reveal concerning the processing of foods. We have concluded that C30 columns provide an excellent separation of structural, geometrical and optical isomers of epoxycarotenoids and that the presence of 5,8-epoxide groups leads to a better shape recognition, to the extent that over 10 geometrical,optical isomers of 5,8-epoxycarotenoids have been separated. Additionally, it was observed that these carotenoids elute later than their 5,6-epoxide counterparts, albeit the latter have a longer chromophore. [source] Preparation of a monolithic column for weak cation exchange chromatography and its application in the separation of biopolymersJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1 2006Yinmao Wei Abstract A procedure for the preparation of a monolithic column for weak cation exchange chromatography was presented. The structure of the monolithic column was evaluated by mercury intrusion. The hydrodynamic and chromatographic properties of the monolithic column , such as back pressures at different flow rates, effects of pH on protein retention, dynamic loading capacity, recovery, and stability , were determined under conditions typical for ion-exchange chromatography. The prepared monolithic column might be used in a relatively broad pH range from 4.0 to 12.0 and exhibited an excellent separation to five proteins at the flow rates of both 1.0 and 8.0 mL/min, respectively. In addition, the prepared column was first used in the purification and simultaneous renaturation of recombinant human interferon gamma (rhIFN-,) in the extract solution with 7.0 mol/L guanidine hydrochloride. The purity and specific bioactivity of the purified rhIFN-, in only one chromatographic step were obtained to be 93% and 7.8×107 IU/mg, respectively. [source] | ||||||||||