Search results for "resolution."
showing 10 items of 1825 documents
Quantitative evaluation of the phenolic profile in fruits of six avocado (Persea americana) cultivars by ultra-high-performance liquid chromatography…
2016
The phenolic profiles of six varieties of avocado (Persea americana) grown in Sicily were investigated. The ultra-high-performance liquid chromatography-heated electrospray-mass spectrometry method was developed to determine qualitative and quantitative changes in fruits at two different ripening stage. Nineteen individual phenolic compounds were detected in avocado pulp extracts. Gallic acid, sinapinic acid, vanillin, p-coumaric acid, and gentisic acid were present only in ripe fruits. On the contrary, epicatechin decreased with fruit ripening, whereas protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, and benzoic acid were relatively stable or exhibited erratic changes with fru…
Prediction of peak shape in hydro-organic and micellar-organic liquid chromatography as a function of mobile phase composition
2007
A simple model is proposed that relates the parameters describing the peak width with the retention time, which can be easily predicted as a function of mobile phase composition. This allows the further prediction of peak shape with global errors below 5%, using a modified Gaussian model with a parabolic variance. The model is useful in the optimisation of chromatographic resolution to assess an eventual overlapping of close peaks. The dependence of peak shape with mobile phase composition was studied for mobile phases containing acetonitrile in the presence and absence of micellised surfactant (micellar-organic and hydro-organic reversed-phase liquid chromatography, RPLC). In micellar RPLC…
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…
Interpretive optimisation strategy applied to the isocratic separation of phenols by reversed-phase liquid chromatography with acetonitrile–water and…
2000
An optimisation protocol is presented for the resolution of complex mixtures in isocratic RPLC with binary mobile phases of organic solvent and water, which is based on the prediction of peak position and shape of the individual compounds. A good description of the retention was achieved through the application of statistical weights to the widely used linear or quadratic relationships between the logarithm of the retention factor (log k) and the organic solvent concentration in the mobile phase. The maximisation of the product of peak purities for each compound is shown as a competitive resolution strategy versus the worst value of a selectivity parameter. Peak purities allow one to associ…
A chromatographic objective function to characterise chromatograms with unknown compounds or without standards available
2015
Abstract Getting useful chemical information from samples containing many compounds is still a challenge to analysts in liquid chromatography. The highest complexity corresponds to samples for which there is no prior knowledge about their chemical composition. Computer-based methodologies are currently considered as the most efficient tools to optimise the chromatographic resolution, and further finding the optimal separation conditions. However, most chromatographic objective functions (COFs) described in the literature to measure the resolution are based on mathematical models fitted with the information obtained from standards, and cannot be applied to samples with unknown compounds. In …
Optimised procedures for the reversed-phase liquid chromatographic analysis of formulations containing tricyclic antidepressants.
2003
The chromatographic behaviour (retention, selectivity, peak shape and resolution) of seven tricyclic antidepressants (TCAs), amitryptiline, clomipramine, doxepin, imipramine, maprotiline, nortryptiline and trimipramine, was examined. Conventional unendcapped Cs and C18 columns and an endcapped XTerra MS C18 column recommended for the analysis of basic compounds were used together with acetonitrile-water and micellar sodium dodecylsulfate (SDS)-pentanol mobile phases. The two best combinations were XTerra C18/acetonitrile, which yielded the largest efficiencies and resolution, and C8/SDS-pentanol, which eliminated the peak tails that were still observed with the XTerra C18 column. Both the s…
Reversed phase liquid chromatography for the enantioseparation of local anaesthetics in polysaccharide-based stationary phases. Application to biodeg…
2020
[EN] A comprehensive study on the chiral separation of bupivacaine, mepivacaine, prilocaine and propanocaine with eight commercial polysaccharide-based chiral stationary phases (CSPs) in reversed phase conditions compatible with MS detection is performed. Methanol and acetonitrile are used as organic modifiers. Retention and resolution values obtained for each compound in the different CSPs and mobile phases are compared. The polysaccharide-based CSPs tested present different enantioselectivity towards the analytes. From the results, the experimental conditions for determining the enantiomers of bupivacaine, mepivacaine, prilocaine and propanocaine in saline aqueous samples using MS detecti…
Short and Efficient Chemoenzymatic Synthesis of Goniothalamin.
2004
A high-yielding three-step synthesis of goniothalamin involving an enzymatic kinetic resolution in the presence of vinyl acrylate followed by ring-closing metathesis is discussed.
VLBI detection of the HST-1 feature in the M87 jet at 2 cm
2010
A bright feature 80 pc away from the core in the powerful jet of M87 shows highly unusual properties. Earlier radio, optical and X-ray observations have shown that this feature, labeled HST-1, is superluminal, and is possibly connected with the TeV flare detected by HESS in 2005. It has been claimed that this feature might have a blazar nature, due to these properties. To examine the possible blazar-like nature of HST-1, we analyzed lambda 2 cm VLBA archival data from dedicated full-track observations and the 2 cm survey/MOJAVE VLBI monitoring programs obtained between 2000 and 2009. Applying VLBI wide-field imaging techniques, the HST-1 region was imaged at milliarcsecond resolution. Here …
ChemInform Abstract: High-Resolution Solid-State NMR Spectroscopy of Steroids and Their Derivatives
2013
Abstract: Steroids are an important class of organic compounds containing a vast array of biologically and physiologically essential molecules. Due to their availability, relatively straightforward derivatizability, and endogeneity, they are widely used in pharmacological applications. The investigation of molecular and physicochemical properties of active pharmaceutical ingredients (APIs) in the solid state is important, because these properties are directly related to their pharmacological activity. Several methods are available for this purpose. Solid-state NMR spectroscopy offers a nondestructive and flexible technique, providing both structural and dynamic information. It can be applie…