Search results for "Elution"
showing 10 items of 337 documents
Approaches to estimate the time and height at the peak maximum in liquid chromatography based on a modified Gaussian model
2011
The time and height at the peak maximum are key parameters to describe a chromatographic peak with prediction or optimization purposes, or in the qualitative/quantitative analysis of samples. Three different approaches to estimate these parameters, using the experimental points in the peak maximum region, are here described and compared. The approaches are based on the reliable description of the peak profile using a modified Gaussian model with a parabolic variance (PVMG). In the first approach, non-linear fitting of the chromatographic data to the PVMG model is carried out to obtain the time and height at the peak maximum (Approach I). In the other two approaches, the PVMG model is linear…
Stationary phase modulation in liquid chromatography through the serial coupling of columns: A review
2016
Liquid chromatography with single columns often does not succeed in the analysis of complex samples, in terms of resolution and analysis time. A relatively simple solution to enhance chromatographic resolution is the modulation of the stationary phase through the serial coupling of columns. This can be implemented with any type of column using compatible elution conditions and conventional instruments. This review describes the key features of column coupling and published procedures, where two or more columns were coupled in series to solve separation problems. In all reports, the authors could not resolve their samples with single columns, whereas significant enhancement in chromatographi…
Retention mechanisms for basic drugs in the submicellar and micellar reversed-phase liquid chromatographic modes.
2008
The reversed-phase liquid chromatographic (RPLC) behavior (retention, elution strength, selectivity, efficiency, and peak asymmetry) for a group of basic drugs (beta-blockers), with mobile phases containing the anionic surfactant sodium dodecyl sulfate (SDS) and acetonitrile, revealed different separation environments, depending on the concentrations of both modifiers: hydro-organic, submicellar at low surfactant concentration and high concentration of organic solvent, micellar, and submicellar at high concentration of both surfactant and organic solvent. In the surfactant-mediated modes, the anionic surfactant layer adsorbed on the stationary phase interacts strongly with the positively ch…
HYDRO-ORGANIC AND MICELLAR-ORGANIC REVERSED-PHASE LIQUID CHROMATOGRAPHIC PROCEDURES FOR THE EVALUATION OF SULPHONAMIDES IN PHARMACEUTICALS
2001
Two reversed-phase liquid chromatographic procedures were developed for the analysis of ten pharmaceutical formulations used in medicine and veterinary, which contained one of the following sulphonamides: sulphacetamide, sulphadiazine, sulphaguanidine, sulphamethazine, sulphamethizole, sulphamethoxazole, or sulphathiazole. In both chromatographic modes, the same C18 column was utilized and the mobile phase contained a low amount of acetonitrile and citric buffer at pH 3.0. In one of the procedures, the surfactant sodium dodecyl sul phate was added to the mobile phase. The presence of micelles allowed a decrease in the amount of organic solvent from 11% to 6%, and facilitated sample dissolut…
Processing of Generator-Produced 68Ga for Medical Application
2007
The (68)Ge/(68)Ga generator provides an excellent source of positron-emitting (68)Ga. However, newly available "ionic" (68)Ge/(68)Ga radionuclide generators are not necessarily optimized for the synthesis of (68)Ga-labeled radiopharmaceuticals. The eluates have rather large volumes, a high concentration of H(+) (pH of 1), a breakthrough of (68)Ge, increasing with time or frequency of use, and impurities such as stable Zn(II) generated by the decay of (68)Ga, Ti(IV) as a constituent of the column material, and Fe(III) as a general impurity.We have developed an efficient route for the processing of generator-derived (68)Ga eluates, including the labeling and purification of biomolecules. Prec…
Glass capillary gas chromatography of chlorinated methyl acetates, propanoates and butanoates on Carbowax 20M and SE-30 columns
1982
The gas chromatography of all chlorinated methyl acetates, methyl propanoates and methyl mono- and dichlorobutanoates has been studied on Carbowax 20M and SE-30 glass capillary columns under various running conditions. The order of elution on a non-polar column was largely determined by the boiling point of esters, whereas on a polar column it was much influenced by the structure of compounds. Complete separation of the combined mixture of all 27 compounds could not be achieved, however, methyl 3,3-dichlorobutanoate was the only ester overlapped on both columns in spite of the various column temperatures used. The best separation of the mixture was on Carbowax 20M with a temperature program…
Synchronized gradient elution in capillary liquid chromatography
2013
Abstract The synchronization of injection valve operation and gradient elution in capillary liquid chromatography (cHPLC) is studied. Focus is placed on the cHPLC systems which rely on the splitting of a primary flow to provide the much smaller secondary flow required at the injection device and analytical column. Owing to the tiny secondary flow rates, synchronization is necessary to achieve proper optimization of gradient elution methods. Otherwise, there is a risk of having the analytes totally or partially eluted in the initial isocratic conditions, and there is no control on the actual gradient profile reaching the column. Synchronization is first achieved by switching back the valve t…
Gas—liquid chromatographic analyses
1984
Abstract The gas choromatographic retention behaviour of veratrole and all nine chlorinated veratroles was studied on SE-30 and OV-351 capillary columns. Temperature programming from 100°C at 6°C min−1 and isothermal operation at 140, 160, 180 and 200°C were used. The complete separation of a mixture was obtained on SE-30, the isomers being eluted in order of their degree of chlorination. On OV-351, however, the 3,4,5-trichloro and tetrachloro isomers overlap with temperature programming, being separated at 140, 160 and 200°C. Retention indices and increments of retention indices for each position of substitution are examined and the effect of increasing temperature on retention is discusse…
Flow Injection Fourier Transform Infrared Determination of Caffeine in Soft Drinks
1997
A fully automated procedure has been developed for FT-IR determination of caffeine in soft drinks. Samples are first degasified by filtration and then directly injected into a flow manifold and passed through a 100 mg C18 SPE cartridge, conditioned with methanol and water. After the cartridge has been cleaned with water, the caffeine is eluted with CHCl3 and stabilized with ethanol. The flow injection (FI) recording is obtained by measuring the absorbance at 1658 cm-1 with a baseline established at 1800 cm-1. Area values for the FI recording obtained between 0.4 and 1.4 min after sample injection are interpolated in the calibration graph of a series of aqueous standards of caffeine, which w…
Evaluation of the representativeness of the odor of beer extracts prior to analysis by GC eluate sniffing
1993
The importance of obtaining and proving that the odor of an extract is representative of the odor of the original product from which it was obtained, before analysis by GC-FID, GC-MS, or GC sniff, is discussed. The sensory methods, such as triangle tests, matching tests, and quantitative analysis, used to determine the representativeness of the odor of an extract are described. Beer extracts obtained by three methods were used to illustrate the interest of the sensory tests. A method using a mixture of XAD resins was proved by sensory analysis to give some extracts with sensory characteristics representative of the particular beers from which they were obtained