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Column Separations (column + separation)
Selected AbstractsSemi-online nanoflow liquid chromatography/matrix-assisted laser desorption ionization mass spectrometry of synthetic polymers using an octadecylsilyl-modified monolithic silica capillary columnRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2010Takehiro Watanabe We have designed a semi-online liquid chromatography/matrix-assisted laser desorption/ionization mass spectrometry (LC/MALDI-MS) system to introduce eluent from a octadecylsilyl (ODS) group modified monolithic silica capillary chromatographic column directly onto a sample plate for MALDI-MS analysis. Our novel semi-online system is useful for rapidly and sensitively examining the performance of a monolithic capillary column. An additional advantage is the small elution volume of a monolithic capillary column, which allows delicate eluents, such as 1,1,1,3,3,3,-hexafluoroisopropyl alcohol (HFIP), to be used to achieve cost-effective analysis. Using the semi-online LC/MALDI-MS system, chromatographic separation of polymers by the monolithic column with different eluents was studied. Separation of poly(methyl methacrylate) and Nylon 6/6 showed that the column functioned via size-exclusion separation when tetrahydrofuran or HFIP eluent was used. On the other hand, the separation behavior of Nylon 11 indicated a reversed-phase mode owing to the interaction of the polymer with the modified ODS group in the column. Using tetrahydrofuran/methanol (1:1, v/v) as the eluent, the LC/MALDI-MS spectra of poly(lactic acid), which contains both linear and cyclic polymer structures, showed that the column could separate the hydrophobic cyclic polymer and elute it out relatively slowly. The monolithic column functions basically via size-exclusion separation; the reversed-phase separation by interaction with the ODS functions may have less influence on column separation. The semi-online monolithic capillary LC/MALDI-MS method we have developed should provide a means of effectively analyzing synthetic polymers. Copyright © 2010 John Wiley & Sons, Ltd. [source] Analytical, Risk Assessment, and Remedial Implications Due to the Co-Presence of Polychlorinated Biphenyls and Terphenyls at Inactive Hazardous Waste SitesREMEDIATION, Issue 1 2000James J. Pagano Investigations conducted at three inactive hazardous waste sites in New York State have confirmed the co-presence of polychlorinated hiphenyls (PCBs) and polychlorinated terphenyls (PCTs) in soils, sediments, and biota. The PCTs at all three sites were positively identified as Aroclor 5432, with the most probable source being the hydraulic fluid Pydraul 312A utilized for high-temperature applications. The identification of the lower-chlorinated PCT formulations in environmental samples is problematical, since PCT Aroclors 5432 and 5442 are not chromatographically distinct from the higher-chlorinated (PCB) Aroclors 1254, 1260, 1262, and 1268 using conventional gas chromatography,electron capture detection. Results from this study indicate that U.S. Environmental Protection Agency (USEPA) approved PCB methods routinely utilized by most commercial laboratories based on Florisil adsorption column chromatography cleanup are inadequate to produce valid chromatographic separation and quantitative results with soils, sediment, and biota samples containing both PCBs and PCTs. The presence of co-eluting PCBs and PCTs precludes accurate quantitation due to significant differences in PCB/PCT electron capture detector response factors, and the potential for misidentification of PCT Aroclors as higher chlorinated PCB Aroclors. A method based on alumina column adsorption chromatography was used, allowing for the accurate identification and quantitation of PCB and PCT Aroclors. The results of this study suggest that the utilization of alumina adsorption column separation may have applicability and regulatory significance to other industrially contaminated sites which historically used Pydraul 312A. Inferences. [source] Validation of theory of n -column separations with gas chromatograms predicted by commercial softwareJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1 2007Yuping Williamson Abstract A probability theory for the average number of compounds resolved by the partial separation of complex mixtures on n columns was tested using commercial-software predictions of gas chromatograms. Such n -column separations are traditional means for addressing peak overlap, in which one chooses additional columns of different selectivity to separate compounds that cannot be separated by a single column. Gas chromatograms of five types of complex mixtures containing from 99 to 283 compounds were predicted for eight stationary phases using both optimized and other temperature programs. The number n of columns for different mixtures varied from 2 to 5. The numbers of compounds separated as singlet peaks at different resolution thresholds were compared to predictions, as evaluated with point-process statistical-overlap theory based on a Poisson distribution. A good agreement between theory and results was found in all cases corresponding to low saturation. Both good and poor agreements were found for cases corresponding to high saturation. A good agreement also was found for results based on resolving complex mixtures by a single column subject to two temperature programs. The moments and distribution of the number of resolved compounds were computed by Monte Carlo simulation, thus gauging the significance of departures between results and theory. The potential of such simulations to explore the limitations of theory was briefly investigated. [source] Capillary columns in liquid chromatography: between conventional columns and microchipsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 17-18 2004Yoshihiro Saito Abstract Liquid chromatography on columns with small internal diameters has been reviewed as the intermediate technique between conventional liquid chromatography and microchip separations. The development of micro column separations in the early years has been described, starting with the papers of Horváth and co-workers and Ishii and co-workers, continuing into the first part of the eighties, then making a leap in time to recent innovations with small-bore columns. Based on internal diameters a classification of the different analytical HPLC columns has been suggested. The advantages of small-bore columns have been discussed, with particular emphasis on the advantage of coupling to concentration sensitive detectors when the sample amount is limited. Open tubular columns are treated as a part of the historic background. The recent developments include a brief look into the current status of monolithic columns, the use of packed nano columns and micro columns with electrospray mass spectrometry, and the potential of two-dimensional comprehensive liquid chromatography. Finally, the coupling of sample preparation to analytical columns and the future applications of the novel technological improvements to the microchip separation methods have been discussed. [source] Ultra-performance liquid chromatography coupled to linear ion trap mass spectrometry for the identification of drug metabolites in biological samplesRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 8 2006G. J. Dear The coupling of ultra-performance liquid chromatography, operating at elevated pressures, to a linear ion trap mass spectrometer provides a high-performance system suitable for drug metabolite characterisation. This system demonstrates improved chromatographic efficiency and sensitivity and at the same time provides diagnostic MSn data often critical for metabolite structural assignment. The linear ion trap was capable of dealing with the high chromatographic efficiencies and hence narrow peak widths associated with 1.7,µm particle-packed column separations. Polarity switching and data-dependent MSn data were generated with ease, and applied to the identification of metabolites found in human plasma. Copyright © 2006 John Wiley & Sons, Ltd. [source] Modeling of Product Removal during Enzymatic Conversions by Using Affinity MoleculesBIOTECHNOLOGY PROGRESS, Issue 6 2007Daniël G. R. Halsema The feasibility of using magnetic particles for in-line product isolation during enzymatic conversion was studied. A comparison was made between a process based on magnetic particles and a conventional adsorption column. The enzymatic reaction was described by two consecutive first-order reactions (synthesis and subsequent hydrolysis), while the adsorption of substrate and product was described by multicomponent Langmuir isotherms. The yield as well as synthesis/hydrolysis ratio were calculated for various system characteristics. The results show that magnetic particles are very effective when the affinity with the particles is specific and for enzymatic conversions involving low ratios of the rate of synthesis versus the rate of hydrolysis. For slow conversions and for low specific affinity molecules column separations are more appropriate. [source] | ||||||||||