Search results for "high-performance liquid chromatography"

Enhanced calculation of optimal gradient programs in reversed-phase liquid chromatography

2003

Abstract The resolution of a mixture of 16 β-blockers under gradient elution was optimised using both isocratic and gradient training sets, with a reversed-phase column and acetonitrile–water eluents. Error theory was applied to measure the information extracted from different gradient experimental designs. This allows checking the expected accuracy when gradient predictions exceed the initial solvent concentrations tested in the training set. This work applies the results on modelling found in a previous study [J. Chromatogr. A 1018 (2003) 169] where the performance of several retention models was compared. Enhanced retention predictions were applied to the optimisation of gradient program…

Peak dispersion in gradient elution: An insight based on the plate model.

2020

Gradient elution in liquid chromatography reduces the analysis time, improves the efficiency and increases the peak capacity. The study of this chromatographic mode has been based mainly on kinetic dispersion models. The plate model has been applied to a lesser extent, despite being the basis for the concepts of plate height and chromatographic efficiency. In this work, a general equation describing peak dispersion in HPLC gradient elution is derived from the plate model. This equation is studied and validated for three types of gradients: (i) a reference gradient without ramp in which the retention factor varies with time identically throughout the column, (ii) a gradient of stationary pha…

Combined effect of solvent content, temperature and pH on the chromatographic behaviour of ionisable compounds.

2008

The organic solvent content and the pH in the mobile phase are the usual main factors in reversed-phase liquid chromatographic separations, owing to their strong effects on retention and/or selectivity. Temperature is often neglected. However, even in cases where the impact of this factor on selectivity is minor, the reduction in analysis time is still an interesting reason to consider it. In addition, ionisable compounds may exhibit selectivity changes, owing to the interaction of organic solvent and/or temperature with pH. The separation of ionisable compounds (nine diuretics: bendroflumethiazide, benzthiazide, bumetanide, chlorthalidone, furosemide, piretanide, probenecid, trichloromethi…

Retention behaviour of volatile compounds in normal-phase high-performance liquid chromatography on a diol column

1993

Abstract Retention data on a diol column for over 300 compounds of the chemical classes usually contained in aroma extracts of plants and foodstuffs are reported. A concept that largely corrects for minor fluctuations of the mobile phase composition and of the flow-rate was used to measure capacity factors. The mobile phase was composed of pentane and diethyl ether. The high volatility of these two solvents makes the method perfectly adaptable to the prefractionation of aroma extracts and the semi-preparative isolation of compounds. Non-polar compounds such as hydrocarbons are not retained on diol. Polar compounds can be readily eluted, with the exception of strong acids and bases.

Passive sampling in monitoring of nonylphenol ethoxylates and nonylphenol in aquatic environments

2012

The present practices for determining the concentration levels of various pollutants are in many respects insufficient and for this reason, there is an urgent need especially to develop more cost-effective sampling methods. In this study, a novel passive sampling tool (the Chemcatcher®) for monitoring nonylphenol ethoxylates (NPEOs) and nonylphenol (NP) in aqueous media was tested. These environmentally harmful substances have been widely used in different household and industrial applications and they affect aquatic ecosystems, for example, by acting as endocrine disrupting compounds. The highest accumulation of NPEOs and NP in laboratory-scale tests was obtained when using an SDB-XC (stan…

Quantitative determination of casein genetic variants in goat milk: Application in Girgentana dairy goat breed

2016

The study was conducted to develop a high-performance liquid chromatographic (HPLC) method to quantify casein genetic variants (αs2-, β-, and κ-casein) in milk of homozygous individuals of Girgentana goat breed. For calibration experiments, pure genetic variants were extracted from individual milk samples of animals with known genotypes. The described HPLC approach was precise, accurate and highly suitable for quantification of goat casein genetic variants of homozygous individuals. The amount of each casein per allele was: αs2-casein A = 2.9 ± 0.8 g/L and F = 1.8 ± 0.4 g/L; β-casein C = 3.0 ± 0.8 g/L and C1 = 2.0 ± 0.7 g/L and κ-casein A = 1.6 ± 0.3 g/L and B = 1.1 ± 0.2 g/L. A good correl…

1996

18:2Δ 9c,12t and 18:2 Δ9t,12c are present in our diet, as result of heat treatment of vegetable oils. A nutritional study was carried out in order to obtain more precise information on the conversion of these two isomers into long chain polyunsaturated fatty acids (PUFA) by rat tissues. This in vivo study performed using rat fed with small quantities of mono trans linoleic acid isomers (0.6% of total energy) showed that 18:2 Δ9c,12t was converted into 20:4 Δ5c,8c,11c,14t while 18:2 Δ9t,12c was only slightly converted into 20:4 Δ5c,8c,11t,14c. Furthermore 18:2 Δ9t,12c was preferentially elongated into 20:2 Δ11t,14c. Each C20 metabolite of these mono trans 18:2 isomers was isolated as methyl …

Cyclodextrins in polymer synthesis: Influence of methylated β-cyclodextrin as host on the free radical copolymerization reactivity ratios of hydropho…

2001

Methylated (β-cyclodextrin (me-β-CD) was used to complex the hydrophobic monomers n-butyl acrylate (1), n-hexyl acrylate (2) and cyclohexyl acrylate (3) yielding the corresponding water soluble host/guest complexes 1a–3a. The complexes were copolymerized in water by free radical mechanism and the reactivity ratios were determined by measuring the monomer consumption by HPLC. The following reactivity ratios were found: copolymerization of 1a and 2a: r1= 1.01 ± 0.01; r2= 1.04 ± 0.01; copolymerization of 3a and 2a: r1= 0.74; r2= 1.28; copolymerization of 3a and 1a: r1= 0.75 ± 0.04; r2= 1.13 ± 0.01. In contrast to that, the copolymerization of the uncomplexed monomers 1–3 in organic medium (DMF…

Isolation and structural characterization of polypeptide antibiotics of the peptaibol class by high-performance liquid chromatography with field deso…

1984

Abstract A number of polypeptide antibiotics of the peptaibol class, i.e., trichotoxin, alamethicin, suzukacillin, hypelcin and paracelsin, have been separated into components and isolated by high-performance liquid chromatography on spherical, porous octadecylsilyl bonded phases. All peptaibols were found to reveal a strong microheterogeneity due to single or multiple amino acid exchange. Most of the closely related and partially isobaric sequence analogue could be resolved using mixed alcohol—water eluents. As demonstrated by the structure analysis of the paracelsins and the main component of trichotoxin A-50, high-performance liquid chromatography with field desorption and fast atom bomb…

Chromatographic peak profile of ionogenic analytes upon elution with unbuffered eluents

1998

Experimental proof of the model was carried out for the separation of benzoic acid on a LiChrospher RP-18 column. The observed chromatographic peak profile coincides with the peak profile predicted by the model. The retention times of the dissociated and non-dissociated species determined by using an appropriate fitting procedure were 2.2 and 4.3 min, respectively. Based on these values, a theoretical peak profile was calculated, demonstrating a close agreement with the experimentally observed peak profile. An unexpectedly large difference was found for the retention times of the dissociated and non-dissociated species calculated by a fitting procedure and those experimentally measured on t…