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showing 10 items of 2426 documents
Development of standard operation procedures for the manufacture of n-octadecyl bonded silicas as packing material in certified reference columns for…
2004
The development of standard operation procedures for the manufacture of a n-octadecyl bonded spherical silica packing from partially condensed tetraethoxysilane as silica source is described. The synthesis comprises five intermediate products and six synthesis steps which were examined according to their reproducibility and robustness. The results led to the optimisation of the manufacturing process for a n-octadecyl bonded silica. Correlations were drawn between the dynamic viscosity of the poly(ethoxy)siloxane (PES), the synthesis parameters, the resulting pore structural properties and particle size distribution of the silicas. Validated procedures were developed to manufacture spherical…
Determination of α-Tocopherol in Plasma by High Performance Liquid Chromatography with Fluorescence Detection and Stability of α-Tocopherol under Dif…
2011
In order to study the clinical effects of the antioxidant alpha-tocopherol (tocofersolan, CAS 30999-06-5) a simple, robust, sensitive and reliable high performance liquid chromatography (HPLC) method using fluorescence detection for the daily measurement of alpha-tocopherol concentration in plasma is described. Several methods of HPLC analysis using fluorescence techniques are published, however, investigations of the stability of alpha-tocopherol during sample preparation under different conditions are relevant in the routine measurements and have to date not been reported. Therefore a modified method, both sensitive and robust, qualified for the day-by-day measurement of alpha-tocopherol …
Combined effect of solvent content, temperature and pH on the chromatographic behaviour of ionisable compounds. III: Considerations about robustness
2009
Abstract We previously reported a model able to predict the retention time of ionisable compounds as a function of the solvent content, temperature and pH [J. Chromatogr. A 1163 (2007) 49]. The model was applied further, developing an optimisation of the resolution based on the peak purity concept [J. Chromatogr. A 1193 (2008) 117]. However, we left aside an important issue: we did not consider incidental overlaps caused by shifts in the predicted peak positions, owing either to uncertainties in the source data, modelling errors, or the practical implementation in the chromatograph of the optimal mobile phase (or any other). These shifts can ruin the predicted separation, since they can eas…
Levels in the interpretive optimisation of selectivity in high-performance liquid chromatography: a magical mystery tour.
2006
Interpretive approaches for selectivity optimisation, which are those supported by retention models, are able to exploit efficiently the capabilities of the chromatographic system. The resolution of a mixture is usually faced in a first trial by looking for a unique experimental condition, able to resolve all compounds in the sample. If this is not possible, the problem can be outlined with less ambitious aims, focusing on only some compounds. In an extreme case, a single analyte can be individually optimised. Current strategies that give answer to the different goals pursued in the analysis, which are classified as total, partial and specific, are reviewed. Optimisation oriented to deconvo…
Comparison of microextraction procedures to determine pesticides in oranges by liquid chromatography-mass spectrometry.
2002
A liquid chromatographic-mass spectrometric method has been developed for the determination of bitertanol, carbendazim, fenthion, flusilazole, hexythiazox, imidacloprid, methidathion, methiocarb, pyriproxyfen and trichlorfon. Two procedures, based on stir bar sorptive extraction (SBSE) and matrix solid-phase dispersion (MSPD), have been evaluated for the extraction of these compounds in oranges. Their respective advantages and disadvantages are also discussed. The recoveries obtained by MSPD ranged from 47 to 96% and the relative standard deviations (RSDs) ranged from 1 to 15%, whereas with the SBSE method the recoveries were between 8 and 84% and the RSDs between 4 and 16%. Although, the l…
Impact of pore structural parameters on column performance and resolution of reversed-phase monolithic silica columns for peptides and proteins
2007
In this work, monolithic silica columns with the C4, C8, and C18 chemistry and having various macropore diameters and two different mesopore diameters are studied to access the differences in the column efficiency under isocratic elution conditions and the resolution of selected peptide pairs under reversed-phase gradient elution conditions for the separation of peptides and proteins. The columns with the pore structural characteristics that provided the most efficient separations are then employed to optimize the conditions of a gradient separation of a model mixture of peptides and proteins based on surface chemistry, gradient time, volumetric flow rate, and acetonitrile concentration. Bo…
Impact of the post-treatment conditions of parent silica on the silanization of n-octadecyl bonded silica packings in reversed-phase high-performance…
2001
Native mesoporous silica beads were subjected to a sequence of post-treatment procedure including hydrochloric acid treatment, calcination and subsequent rehydroxylation. The post-treated silica beads were converted into RP-18 silica by silanization with monochloro- and dimethoxy-n-octadecylsilanes, respectively. The influence of post-treatments and silanization conditions on the physico-chemical characteristics and on the chromatographic behaviour of the RP-silicas was studied. Also the changes of the pore structural parameters and the silanol group densities during the post-treatment and silanization were assessed.
Rapid and simultaneous high-performance liquid chromatography assay of polyamines and monoacetylpolyamines in biological specimens
2000
A rapid, resolutive and reproducible reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for polyamines and acetylpolyamines by adopting pre-column derivatization with benzoyl chloride. In a single run lasting less than 15 min ten polyamines were separated as well as traces of benzoic acid, methylbenzoate and benzoic anhydride. These contaminants, produced during the derivatization reaction, were almost all eliminated by washing steps envisaged in the same procedure. This simple and sensitive method can be applied to routine determination of polyamines in biological samples. A fine application of this procedure to the determination of endogenous content of p…
Premature aging in bone of fish from a highly polluted marine area
2015
Fish species have attracted considerable interest in studies assessing biological responses to environmental contaminants. In this study, the attention has been focussed on fishbone of selected fish species from a highly polluted marine area, Augusta Bay (Italy, Central Mediterranean) to evaluate if toxicant elements had an effect on the mineralogical structure of bones, although macroscopic deformations were not evident. In particular, an attempt was made to evaluate if bone mineral features, such as crystallinity, mineral maturity and carbonate/phosphate mineral content, determined by XR-Diffraction and FT-IR Spectroscopy, suffered negative effects due to trace element levels in fishbone,…
Application of Dopant-Assisted Atmospheric Pressure Photoionisation HPLC–MS Method for the Sensitive Determination of Polycyclic Aromatic Hydrocarbon…
2017
Multiple food research studies have shown that the polycyclic aromatic hydrocarbon (PAHs) are frequently found in processed cocoa products and chocolate. In a present study a method based on dopant-assisted atmospheric pressure photoionisation (DA-APPI) combined with a liquid chromatography/high-resolution mass spectrometer (HPLC-HRMS) for high-sensitivity analysis of four EU marker PAHs in dark chocolate samples was developed and fully validated according to the performance criteria set in EU guidelines. PAHs detection was achieved by HRMS in positive electrospray ionization mode with toluene used as a dopant to enhance the ionization efficiency of non-polar PAHs. The on-column instrument …