Search results for "Elution"
showing 10 items of 337 documents
Optimization of Labeling PSMAHBED with Ethanol-Postprocessed 68Ga and Its Quality Control Systems
2017
Radiolabeling of the prostate-specific membrane antigen (PSMA) inhibitor Glu-NH-CO-NH-Lys(Ahx) using the 68Ga chelator HBED-CC (PSMAHBED) allows imaging of prostate cancer lesions because of high expression of PSMA in prostate carcinoma cells and in bone metastases and lymph nodes related to the disease. The aim of this work was to optimize labeling of 68Ga-PSMAHBED using the efficient cation-exchange postprocessing of 68Ga as well as the development of a thin-layer chromatography (TLC)-based quality control system. Methods: Labeling was optimized for online ethanol-postprocessed 68Ga eluate investigating various parameters, such as buffer molarity (0.1-1 M), temperature (25°C-90°C), tracer…
Interpretive optimisation of organic solvent content and flow-rate in the separation of β-blockers with a Chromolith RP-18e column
2009
The chromatographic performance of a Chromolith RP-18e column was comprehensively examined for a group of basic drugs (beta-blockers), eluted with isocratic ACN-water mixtures at increasing flow-rate up to 6 mL/min. As the flow-rate increases at fixed mobile phase composition, peak distribution (selectivity) is maintained, but the relative peak widths increase. This reduces the resolution below satisfactory values for closely eluting compounds. With the monolithic column, flow-rate becomes thus an important factor to be optimised, in addition to the mobile phase composition. Since, theoretically, retention factors (k) are independent of the flow-rate, the classical quadratic model relating …
Impact of pore structural parameters on column performance and resolution of reversed-phase monolithic silica columns for peptides and proteins
2007
In this work, monolithic silica columns with the C4, C8, and C18 chemistry and having various macropore diameters and two different mesopore diameters are studied to access the differences in the column efficiency under isocratic elution conditions and the resolution of selected peptide pairs under reversed-phase gradient elution conditions for the separation of peptides and proteins. The columns with the pore structural characteristics that provided the most efficient separations are then employed to optimize the conditions of a gradient separation of a model mixture of peptides and proteins based on surface chemistry, gradient time, volumetric flow rate, and acetonitrile concentration. Bo…
Isolation and concentration of organophosphorus pesticides from water using a c18 reversed phase
1989
Abstract A simple, rapid and effective method for the extraction and enrichment of organophosphorus pesticides based on the use of Sep-Pak C 18 cartridges was studied as alternative method to those based on extraction with organic solvents. The influence of the elution solvent, pH, salinity and volume of water filtered was studied for ten organophosphorus pesticides. The pesticides were determined by gas chromatography with a BP-1 capillary column and a thermionic detector. Recoveries at the 100 and 200 ng/1 spiking levels were greater than 85%, except for disulfoton.
Solid-Phase Extraction of Organochlorine Pesticides from Water Samples
1990
Abstract A procedure for the accumulation of organochiorine pesticides by reversed-phase adsorption on octadecylsilica glass microcolumns was used for the isolation and concentration from spiked distilled and natural waters. The pesticides were eluted from the octadecylsilica with light petroleum, and analyzed by gas chromatography using an electron capture detector. The average recovery was over 90% in spiked water samples at 0.1 ng/ml. The performance of the octadecylsilica when applied to the analysis of water samples were compared with the Rodier and the APHA solvent extraction methods.
Optimization of the phase system in the analysis of polynuclear aromatics (PNA) from diesel engine exhaust by high performance liquid chromatography …
1979
Polynuclear aromatics (PNA) were collected and enriched from diesel engine exhausts by means of a probe and an absorber system. Group separation of PNA from other constituents of exhaust was accomplished through elution with n-heptane on a silica column. A variety of phase systems ranging from unpolar to strong polar packings and eluents, respectively, were tested to resolve PNA into single species. Of these a n-octadecyl bonded silica packing and methanol/water was found to be the most optimal with regard to resolution for real PNA mixtures. Separation was completed within 2–3 h at isocratic conditions.
Limits of multi-linear gradient optimisation in reversed-phase liquid chromatography
2005
Abstract The concept of limiting peak purity was applied to quantify the degree of completion of the separation capability of a chromatographic system using multi-linear gradients. The objective was to check whether the complexity of a gradient program deserves be increased to enhance resolution by inserting more linear segments, or on the contrary, no significant improvements can be expected under more complex gradients. A set of 19 isoindole derivatives of primary amino acids was selected to test the performance of isocratic, single linear and multi-linear gradients. Accurate simulated chromatograms were obtained via numerical integration of the general equation of gradient elution, using…
Models and objective functions for the optimisation of selectivity in reversed-phase liquid chromatography.
2006
Interpretive methodologies are the most efficient tools for finding the optimal conditions in chromatography. These methodologies are supported by models or algorithms able to infer the system behaviour upon changes in the experimental factors. Once the models are built with data obtained from sets of carefully designed experiments, molecular modelling or other approaches, they can be applied to predict the performance of new conditions. The different elements involved in these methodologies, for both isocratic and gradient elution, are given. Special attention is devoted to the description of retention, owing to its major impact on the prediction of chromatographic resolution. Several mode…
Evaluation of several global resolution functions for liquid chromatography
1999
Abstract An interpretative approach, that makes use of the overlapped fraction of each chromatographic peak as elementary resolution criterion, was applied to the separation of mixtures of compounds. The elementary resolution measurements for all peaks in the chromatogram were reduced to a single numerical value using several functions: normalised by the mean resolution product, unnormalised product, geometrical mean of the unnormalised product, and worst elementary resolution value. The descriptive capability of these reduction functions was evaluated through the observation of global resolution diagrams and the change in the shape of the chromatograms in the selected factor space. michrom…
Resolution of inherently chiral resorcarene derivatives by enantioselective HPLC
1999
Abstract The HPLC enantiomeric resolution of five inherently chiral tetrabenzoxazine derivatives of resorcarenes has been achieved by HPLC using Whelk-Ol and in one case Chiralpak AD as stationary phases. Enantiomeric separation was only observed in a very narrow range of mobile phase compositions. On-column enantiomeric interconversion of a racemic compound with a typical plateau-like elution profile was observed using a Chiralpak AD column