Search results for "Column chromatography"

Automated pre-column derivatization of amines in biological samples with dansyl chloride and with or without post-column chemiluminescence formation …

1999

On-line automation of two different liquid chromatographic procedures, a pre-column derivatization system and a pre- and post-column system, in order to generate chemiluminescence is reported. Dansyl chloride (Dns-Cl) was used as a pre-column reagent to form fluorophores and bis(2,4,6-trichlorophenyl) oxalate (TCPO) and hydrogen peroxide (H2O2) as a post-column reagent to generate chemiluminescence. This procedure is based on the employment of a primary column packed with C18 material inserted in a multi-dimensional assembly for sample clean-up and derivatization with Dns-Cl. The dansyl derivatives formed are transferred and separated in a LiChrospher 100 RP18 analytical column (125 x 4 mm …

Influence of temperature on the behaviour of small linear peptides in capillary electrochromatography

2000

The influence of temperature, T, on the retention times, peak widths, peak symmetry coefficients and theoretical plate numbers of two small linear peptides, [Met5]enkephalin and [Leu5]enkephalin, has been studied with capillary electrochromatography (CEC) capillary columns of 100 microm I.D. and 250 mm packed length with a total length of 335 mm, containing 3 microm Hypersil n-octadecyl bonded silica. With increasing column temperature from 15 to 60 degrees C, the electroosmotic flow (EOF) and the column efficiencies increased, whereas the retention coefficients (Kcec) of both peptides decreased. A linear relationship was found between the EOF value and the square root of the temperature ov…

Highly efficient separation of amines by electrokinetic chromatography using resorcarene-octacarboxylic acids as pseudo-stationary phases

1998

Abstract Resorcarene-octacarboxylic acids, macrocyclic molecules built up by four alkylidene-bridged resorcinol units, were synthesized and used as pseudostationary phases in electrokinetic chromatography (EKC). Resorcarenes provide a stable structure and good solubility in electrolytes even with organic modifiers. The high electrophoretic mobility of the resorcarene-octacarboxylic acids introduced here as pseudostationary phases is based on the eight partly deprotonated carboxylic groups. This offers a broad migration time window, which is the main parameter for the resolution of peaks. From three compounds with different alkyl chain lengths (C 1 , C 5 , C 11 ), the C 11 -resorcarene-octa-…

On-line gradient liquid chromatography–Fourier transform infrared spectrometry determination of sugars in beverages using chemometric background corr…

2008

Abstract An on-line gradient reversed phase liquid chromatography–Fourier transform infrared spectrometry (LC–FTIR) method was developed for the determination of fructose, glucose, sucrose and maltose in beverages. Improved chromatographic resolution was obtained using a linear gradient from 75 to 55% (v/v) acetonitrile in water in 15 min. Changes in the background spectra were corrected employing “univariate background correction based on the use of a reference spectra matrix” (UBC-RSM) and using the ratio of absorbance (AR) at 2256 and 2253 cm −1 for the identification of the eluent spectra within the RSM. The method provided limits of detection in the order of 0.75 mg ml −1 . The precisi…

Absolute optical chiral analysis using cavity-enhanced polarimetry

2021

Chiral analysis is central for scientific advancement in the fields of chemistry, biology, and medicine. It is also indispensable in the development and quality control of chiral compounds in the chemical and pharmaceutical industries. Current methods for chiral analysis, namely optical polarimetry, mass spectrometry and nuclear magnetic resonance, are either insensitive, have low time resolution, or require preparation steps, and so are unsuited for monitoring chiral dynamics within complex environments: the current need of both research and industry. Here we present the concept of absolute optical chiral analysis, as enabled by cavity-enhanced polarimetry, which allows for accurate unambi…

Enantiomer Separations Using Designed Imprinted Chiral Phases

2003

Total Synthesis of (±)-Oxalicumone C and Chiral Resolution and Elucidation of Its Absolute Configuration

2014

The racemic total synthesis, the chiral resolution, and the elucidation of the absolute configuration of the natural product oxalicumone C were investigated. The goal was achieved by a synthetic strategy beginning with the synthesis of a 5-hydroxy-7-methylchromone precursor. Further modification possibilities were achieved by introduction of a vinyl moiety into the chromone, which was based on a selective iodination step in the 3-position. Further transformations furnished the racemic natural product. To determinate the absolute configuration of naturally occurring oxalicumone C, both enantiomers were separated by chiral HPLC. Comparison of the calculated and experimental vibrational circul…

BONDED SILICA PHASES FOR THE SEPARATION OF BIOPOLYMERS BY MEANS OF COLUMN LIQUID CHROMATOGRAPHY

1988

Is multidimensional high performance liquid chromatography (HPLC) an alternative in protein analysis to 2D gel electrophoresis?

2000

The interactive modes of High Performance Liquid Chromatography (HPLC) of proteins provide a platform for the construction of a multidimensional HPLC system coupled to mass spectrometry. We present a system composed of both anion and cation exchanger columns, in the first dimension, and n-octadecyl bonded 1.5 μm nonporous silica columns in the second dimension. Both columns are operated under gradient conditions. A system suitability test with standard proteins showed that the total analysis can be performed within about 20 minutes. The fractions taken from the ion exchanger column are directly analyzed within one minute on the reversed phase column at a high flow rate. Two reversed phase c…

Phase-distribution chromatography (PDC) of polystyrene

1970

A chromatographic technique is described where the stationary phase is a layer of a very high molecular polystyrene fraction (M = 107) on glass beads (ballotines). The mobile phase is cyclohexane passing the column at a constant temperature below the theta-temperature. A polystyrene sample of sufficiently low molecular weight (M ≤ 106) injected as a small plug at the top of the column is fractionated because the distribution between the mobile and the stationary phase depends on the molecular weight. Since the large molecules preferentially remain in the stationary phase, the smaller molecules leave the column first. The fractionation effect is inverse to that found in GPC experiments. The …