Search results for "Elution"
showing 10 items of 337 documents
In vitro bioactive properties of phlorotannins recovered from hydrothermal treatment of Sargassum muticum
2016
Abstract The present work addresses the potential of different adsorbents for the recovery of the phlorotannin fraction present in the liquid phase from the autohydrolysis of Sargassum muticum. Operating with the extract generated during autohydrolysis of alginate exhausted algae, the kinetics followed pseudo-second order and the equilibrium corresponded to Freundlich model. In batch configuration, up to 70% phlorotannins were adsorbed and up to 30% were desorbed with ethanolic solutions. Comparable performance was observed with the autohydrolysis extracts from the whole algae. The phloroglucinol content, the reducing and ABTS antiradical capacities of the desorbed product increased by 2–4 …
Chromatographic separation and partial identification of glycosidically bound volatile components of fruit
1990
Abstract Synthetic monoterpenic and aromatic β- d -glucosides and β- d -rutinosides were separated by Fractogel TSK HW-40 S chromatography according to their molecular size and interactions occurring between the aglycone moiety and the gel matrix. Under these conditions terpenyl rutinosides were eluted before the homologous glucoside derivatives. In the two classes, monoglucosides and rutinosides, aromatic glycosidically bound components had lower retention times than the corresponding terpenyl components. The use of over-pressure layer chromatography (OPLC) allowed the separation of glucoside and rutinoside derivatives, and in these two classes aromatic and several monoterpene compounds we…
A UHPLC-UV Method to Quantify Skin Deposition and Transdermal Permeation of Tizanidine Hydrochloride
2015
Tizanidine hydrochloride is an α2-adrenergic agonist used for the symptomatic relief of spasticity associated with multiple sclerosis or with spinal cord injury or disease. The objective of this study was to develop an isocratic, robust and sensitive ultra-high performance liquid chromatography method using UV detection for use in a project to develop a transdermal therapeutic system to deliver tizanidine across the skin. Isocratic separation was achieved using a C18 column and a mobile phase comprising a 80:20 mixture of 0.004% trifluoroacetic acid in water and MeCN (pH* 3.2) at a flow rate of 0.2 mL min(-1) Tizanidine eluted at 1.499 min and the total run time was 2 min. The method was sp…
Isocratic high-performance liquid chromatographic determination of tryptophan in infant formulas.
1996
The application to infant formulas of a method for tryptophan determination by isocratic HPLC with UV detection at 254 nm, after derivatization with phenyl isothiocyanate, was studied. Protein was hydrolysed by barium hydroxide at 120 degrees C for 8 h, followed by derivatization with phenyl isothiocyanate, HPLC and UV detection at 254 nm. The optimum chromatographic conditions (pH, ionic strength of elution solvent and eluent ratio) were established. The analytical parameters (linearity, precision, accuracy of derivatization and limits of detection and quantification) were determined. The values obtained demonstrated that the method is useful for determining the tryptophan content of infan…
Effect of short-chain alcohols on surfactant-mediated reversed-phase liquid chromatographic systems.
2010
The behaviour of β-blockers in a reversed-phase liquid chromatographic (RPLC) column with mobile phases containing a short-chain alcohol (methanol, ethanol or 1-propanol), with and without the surfactant sodium dodecyl sulphate (SDS), was explored. Two surfactant-mediated RPLC modes were studied, where the mobile phases contained either micelles or only surfactant monomers at high concentration. Acetonitrile was also considered for comparison purposes. A correlation was found between the effects of the organic solvent on micelle formation (monitored by the drop weight procedure) and on the nature of the chromatographic system (as revealed by the retention, elution strength and peak shape of…
Submicellar and micellar reversed-phase liquid chromatographic modes applied to the separation of beta-blockers.
2009
The behaviour of a reversed-phase liquid chromatographic (RPLC) system (i.e. elution order, resolution and analysis time), used in the analysis of β-blockers with acetonitrile-water mobile phases, changes drastically upon addition of an anionic surfactant (sodium dodecyl sulphate, SDS). Surfactant monomers cover the alkyl-bonded phase in different extent depending on the concentration of both modifiers, in the ranges 1 × 10-3-0.15 M SDS and 5-50% acetonitrile. Meanwhile, the surfactant is dissolved in the mobile phase as free monomers, associated in small clusters or forming micelles. Four characteristic RPLC modes are yielded, with transition regions between them: hydro-organic, micellar, …
Performance of different C18 columns in reversed-phase liquid chromatography with hydro-organic and micellar-organic mobile phases
2014
Column selection in reversed-phase liquid chromatography (RPLC) can become a challenge if the target compounds interact with the silica-based packing. One of such interactions is the attraction of cationic solutes to the free silanols in silica-based columns, which is a slow sorption-desorption interaction process that gives rise to tailed and broad peaks. The effect of silanols is minimised by the addition of a competing agent in the mobile phase, such as the anionic surfactant sodium dodecyl sulphate (SDS). In micellar-organic RPLC, the adsorption of an approximately fixed amount of SDS monomers gives rise to a stable modified stationary phase, with properties remarkably different from th…
Comparative study of solvation parameter models accounting the effects of mobile phase composition in reversed-phase liquid chromatography
2007
Solvation parameter models relate linearly compound properties with five fundamental solute descriptors (excess molar refraction, dipolarity/polarizability, effective hydrogen-bond acidity and basicity, and McGowan volume). These models are widely used, due to the availability of protocols to obtain the descriptors, good performance, and general applicability. Several approaches to predict retention in reversed-phase liquid chromatography (RPLC) as a function of these descriptors and mobile phase composition are compared, assaying the performance with a set of 146 organic compounds of diverse nature, eluted with acetonitrile and methanol. The approaches are classified in two groups: those t…
Performance of a Chromolith RP-18e column for the screening of β-blockers
2009
The chromatographic performance of a monolithic column (Chromolith RP-18e) was comprehensively examined in the isocratic separation of ten beta-blockers, using ACN-water mobile phases, and compared with the performance of three microparticulate RP columns manufactured with different types of silica: Spherisorb ODS-2, Kromasil C18 and XTerra MS C18. The comparison considered the analysis time, selectivity, peak shape (column efficiency and asymmetry) and resolution, and was extended to a wide range of mobile phase compositions. The Chromolith column showed good performance for the analysis of beta-blockers with regard to the packed columns. In terms of selectivity and analysis time, the grea…
A comparative study of the performance of acetonitrile and methanol in the multi-linear gradient separation of proteic primary amino acids
2006
The performance of the separation of proteic primary amino acids using multi-linear gradients of acetonitrile and methanol was studied under an experimental-design basis, using an Inertsil ODS-3 column and pre-column derivatization with o-phthaldialdehyde (OPA) and N-acetyl-l-cysteine (NAC). Elution strength, peak properties, resolution, and analysis time, were examined. The optimal separation was established through modeling, using information obtained from isocratic data. By optimizing the separation with gradients of increasing complexity, acceptable resolution was possible, being glycine/threonine the critical pair. Multi-criteria decision-making (Derringer desirabilities) was applied t…