Search results for "Alkylbenzenes"
showing 9 items of 9 documents
Anionic-anionic asymmetric tandem reactions: one-pot synthesis of optically pure fluorinated indolines from 2-p-tolylsulfinyl alkylbenzenes.
2008
Effect of sodium dodecyl sulphate and Brij-35 on the analysis of sulphonamides in physiological samples using direct injection and acetonitrile gradi…
2016
Micellar liquid chromatography (MLC) is a reversed-phase (RP) mode, which often does not require gradient elution, since the peaks of mixtures of compounds within a large range of polarities appear more evenly distributed in the chromatograms of isocratic elution, giving rise to a “gradient effect”. However, the use of a gradient of organic solvent may still be convenient to shorten the total analysis time. This work compares the separation of 15 sulphonamides using conventional hydro-organic RPLC and MLC with the surfactants sodium dodecyl sulphate (SDS) and Brij-35, and both isocratic and gradient elution with acetonitrile. The observed behaviour is rationalized attending to the interacti…
Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography
2017
[EN] In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch®), or mixtures of H2O2 and H2SO4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification…
Benzyl ions from 1,1-(2,2′-dimethoxyphenyl)-substituted 2-methylpropanes under electron ionization
2006
The electron ionization (EI)-induced fragmentations of a series of 1,1-(2,2'-dimethoxyphenyl)-substituted 2-methylpropanes (1-20) in both 70 eV and mass-analyzed ion kinetic energy (MIKE) spectra have been investigated. The EI-MS spectra of these compounds are characterized by the presence of abundant benzyl ions. These ions result from competitive hydrogen migration from the 2- and 2'-methoxy groups on the carbenium center of the diphenylmethyl cations formed by benzylic cleavage of the molecular ions. The relative abundances of the benzyl ions arising from such competitive processes are discussed and rationalized. The steric effect of the 3- or 3'-substituents is the main discriminating f…
Photo-polymerized lauryl methacrylate monolithic columns for CEC using lauroyl peroxide as initiator
2009
Lauryl methacrylate (LMA)-ester based monolithic columns photo-polymerized using lauroyl peroxide (LPO) as initiator were prepared, and their morphological and CEC properties were studied. The composition of the polymerization mixture (i.e. ratios of monomers/porogenic solvents, 1,4-butanediol/1-propanol and LMA/crosslinker) was optimized. The morphological and chromatographic properties of LMA columns were evaluated by means of SEM pictures and van Deemter plots of PAHs, respectively. The polymerization mixture selected as optimal provided a fast separation of a mixture of PAHs with excellent efficiencies (minimum plate heights of 8.9-11.1 μm). Satisfactory column-to-column (RS D < 4.5%) a…
Life-time studies with capillary electrochromatography columns operated under different conditions.
2000
A test system has been established to permit the monitoring of the life-time performance of several reversed- phase capillary electrochromatography (CEC) columns. The retention factors, k(cec), peak symmetry coefficients, lambda(sym), and column efficiencies, N, of three neutral n-alkylbenzene analytes, namely ethyl-, n-butyl- and n-pentylbenzenes, were determined for Hypersil 3 microm n-octylsilica and n-octadecylsilica packed into CEC capillary columns of 100 microm I.D., with a packed length of 250 mm, and a total length of 335 mm. The performances of these CEC capillary columns were examined for a variety of eluents with pH values ranging between pH 2.0 - 8.0, similar to those employed …
Modelling retention and peak shape of small polar solutes analysed by nano-HPLC using methacrylate-based monolithic columns.
2019
Abstract The development of methacrylate-based monolithic columns was studied for the separation of pharmaceutical hydrophilic compounds in nano-liquid chromatography. The selected polymerisation mixture consisted of 7.5% hexyl methacrylate, 4.5% methacrylic acid and 18.0% ethylene dimethacrylate (w/w), in a binary porogenic solvent (35:35 w/w 1-propanol/1,4-butanediol). The polymer synthesised with this mixture has a good permeability, not excessive back-pressure, and reasonable retention times for polar and non-polar solutes. Monolithic columns (12 cm total capillary length, 100 μm i.d.), prepared with this mixture, were able to produce hydrogen bonding and electrostatic interactions, giv…
Comparative study on the column performance of microparticulate 5-μm C18-bonded and monolithic C18-bonded reversed-phase columns in high-performance …
1999
In this paper we report on the results of a comparative study on the performance of Purospher RP 18e, 5 μm, columns and prototypes of monolithic columns named SilicaROD from Merck, Darmstadt, Germany. The studies were performed on HPLC equipment with minimum extra column contribution. The plate height linear velocity dependency of the Purospher RP 18e column showed a minimum of H of about 10–15 μm at a linear velocity of 1 mm/s. The H versus u curves of the monolithic columns followed the same course. Yet, the curves remained flat up to a linear velocity of about 7 mm/s, where the Purospher RP 18e column could not be operated anymore due to the extremely high back-pressure. In conclusion th…