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Reversed-phase Mode (reversed-phase + mode)
Selected AbstractsMulti-walled carbon nanotube composites with polyacrylate prepared for open-tubular capillary electrochromatographyELECTROPHORESIS, Issue 19 2010Jian-Lian Chen Abstract A new phase containing immobilized carbon nanotubes (CNTs) was synthesized by in situ polymerization of acid-treated multi-walled CNTs using butylmethacrylate (BMA) as the monomer and ethylene dimethacrylate as the crosslinker on a silanized capillary, forming a porous-layered open-tubular column for CEC. Incorporation of CNT nanomaterials into a polymer matrix could increase the phase ratio and take advantage of the easy preparation of an OT-CEC column. The completed BMA-CNT column was characterized by SEM, ATR-IR, and EOF measurements, varying the pH and the added volume organic modifier. In the multi-walled CNTs structure, carboxylate groups were the major ionizable ligands on the phase surface exerting the EOF having electroosmotic mobility, 4.0×104,cm2,V,1,S,1, in the phosphate buffer at pH 2.8 and RSD values (n=5), 3.2, 4.1, and 4.3%, for three replicate capillaries at pH 7.6. Application of the BMA-CNT column in CEC separations of various samples, including nucleobases, nucleosides, flavonoids, and phenolic acids, proved satisfactory upon optimization of the running buffers. Their optima were found in the borate buffers at pH 9.0/50,mM, pH 9.5/10,mM/50% v/v ACN, and pH 9.5/30,mM/10% v/v methanol, respectively. The separations could also be used to assess the relative contributions of electrophoresis and chromatography to the CEC mechanism by calculating the corresponding velocity and retention factors. Discussions about interactions between the probe solutes and the bonded phase included the ,,, interactions, electrostatic repulsion, and hydrogen bonding. Furthermore, a reversed-phase mode was discovered to be involved in the chromatographic retention. [source] Determination of chiral ratio of o,p -DDT and o,p -DDD pesticides on polysaccharides chiral stationary phases by HPLC under reversed-phase modeENVIRONMENTAL TOXICOLOGY, Issue 4 2002Imran Ali Abstract A simple and reliable HPLC method for the chiral resolution of o,p -DDT and o,p -DDD is described. The enantiomeric resolution of o,p -DDT and o,p -DDD has been achieved on Chiralpak AD-R, Chiralcel OD-R, and Chiralcel OJ-R chiral stationary phases. The mobile phases used were acetonitrile,water (50:50 [v/v]) and acetonitrile-2-propanol (50:50 [v/v]) at a flow rate of 1.0 mL/min. For both pesticides detection was done at 220 nm. The values for o,p -DDT of , and Rs varied from 1.24 to 2.52 and from 0.80 to 2.47, respectively. The values of , and Rs for o,p -DDD were 1.26 and 0.60, respectively. © 2002 Wiley Periodicals, Inc. Environ Toxicol 17: 329,333, 2002; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/tox.10069 [source] Semi-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] High-performance liquid chromatography assays for desmethoxyyangonin, methysticin, kavain and their microsomal metabolitesBIOMEDICAL CHROMATOGRAPHY, Issue 1 2009Shuang Fu Abstract Three novel, simple and reproducible high-performance liquid chromatography quantitative assays with UV detection were developed and validated for three major kavalactones,desmethoxyyangonin, methysticin and kavain,in rat liver microsomes using diazepam as an internal standard; liquid,liquid extraction was used for sample preparation and analysis was performed on a Shimadzu® 10A high-performance liquid chromatography system. The analysis was carried out in reversed-phase mode with a Luna® C18 column (150 × 2.00 mm, 3 µm) at 40°C. The limit of quantitation was 0.1 µg/mL using 0.25 mL of microsomal solution. The assays were linear over the range 0.1,10 µg/mL for desmethoxyyangonin, methysticin and kavain. Quality control samples exhibited good accuracy and precision with relative standard deviations lower than 15% and recoveries between 85 and 105%. The assays exhibited satisfactory performance with high sensitivity for quantifying desmethoxyyangonin, methysticin and kavain in rat liver microsomes and were successfully used to determine the three kavalactones and their microsomal metabolites. Copyright © 2008 John Wiley & Sons, Ltd. [source] Column selection and method development for the separation of nucleoside phosphotriester diastereoisomers, new potential anti-viral drugs.BIOMEDICAL CHROMATOGRAPHY, Issue 6 2005Application to cellular extract analysis Abstract Analytical HPLC methods using derivatized cellulose and amylose chiral stationary phases used in normal and reversed-phase modes were developed for the diastereoisomeric separation of mononucleotide prodrugs (pronucleotides) of 3,-azido-2,,3,-dideoxythymidine (AZT). The resolutions were performed with two silica-based celluloses using normal and reversed-phase methodologies: Tris-3,5-dimethylphenylcarbamate (Chiralcel OD-H and Chiracel OD-RH) and Tris-methylbenzoate (Chiralcel OJ and OJ-R). Two amyloses phases, Tris-3,5-dimethylphenylcarbamate (Chiralpak AD) and Tris-(S)-1-phenylethylcarbamate (Chiralpak AS), were used in normal-phase mode. Additionally, we developed separation using two stationary phases with immobilized cyclodextrins in reversed-phase and polar-organic modes. The mobile phase and the chiral stationary phase were varied to achieve the best resolution. Different types and concentration of aliphatic alcohols, acetonitrile or water in the mobile phase were also tested for the different separation modes. An optimal baseline separation (Rs > 1.5) was readily obtained with all silica-based celluloses and amyloses using a normal-phase methodology. The different columns gave complementary results in term of resolution. Limits of detection and quantification were 0.12,0.20 and 0.40,0.67 µm, respectively. This analytical method was applied in a preliminary study for the pronucleotide 2 quantification in cellular extract. Copyright © 2005 John Wiley & Sons, Ltd. [source] 5-Alpha- and 5-beta-2-deoxyintegristerone A, a 5-alpha and 5-beta isomer pair of ecdysteroids isolated from the Silene genusBIOMEDICAL CHROMATOGRAPHY, Issue 6 2002M. Báthori 5-Alpha-2-deoxyintegristerone A and 5-beta-2-deoxyintegristerone A were isolated from the aerial parts of Silene italica ssp. nemoralis (Waldst. and Kit.) Nyman using a specific combination of absorption column chromatography, preparative thin-layer chromatography and preparative HPLC. Both normal-phase and reversed-phase modes of HPLC were employed for isolation. Structural elucidation of 5-alpha-2-deoxyintegristerone A was completed by X-ray diffraction. Both 5-alpha-2-deoxyintegristerone A and 5-beta-2-deoxyintegristerone A were firstly isolated from this plant. We propose that 5-alpha-2-deoxyintegristerone A is not an artifact but an integral part of the ecdysteroid spectrum of Silene italica ssp. nemoralis (Waldst. and Kit.) Nyman. Copyright © 2002 John Wiley & Sons, Ltd. [source] | ||||||||||