Search results for "solution"
showing 10 items of 5638 documents
o-Phthalaldehyde–N-acetylcysteine polyamine derivatives: formation and stability in solution and in C18 supports
2001
A comparative study of different derivatization procedures has been performed in order to improve the stability of the reaction products o-phthalaldehyde-N-acetylcysteine (OPA-NAC) polyamines. Procedures such as solution derivatization, solution derivatization followed by retention on a packing support, derivatization on different packing supports and on-column derivatization, have been optimized and compared. The degradation rate constant (k) of the derivative was dependent on the procedure used and on the analyte. For the spermine (the most unstable isoindol tested) k was 8 +/- 2 x 10(-2) min(-1) in solution versus 7.7 +/- 1.1 x 10(-4) min(-1) on the (C18) solid support. The results obtai…
Green aspects, developments and perspectives of liquid phase microextraction techniques.
2014
Determination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte isolation/enrichment prior to analysis is required in many cases. In this work the newest trends and innovations in liquid phase microextraction, like: single-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liqu…
Optimisation of gradient elution with serially-coupled columns. Part I: single linear gradients.
2014
A mixture of compounds often cannot be resolved with a single chromatographic column, but the analysis can be successful using columns of different nature, serially combined through zero-dead volume junctions. In previous work (JCA 1281 (2013) 94), we developed an isocratic approach that optimised simultaneously the mobile phase composition, stationary phase nature and column length. In this work, we take the challenge of implementing optimal linear gradients for serial columns to decrease the analysis time for compounds covering a wide polarity range. For this purpose, five ACE columns of different selectivity (three C18 columns of different characteristics, a cyano and a phenyl column) we…
Application of solid-phase microextraction combined with derivatization to the enantiomeric determination of amphetamines.
2005
Abstract The utility of combining chiral derivatization and solid-phase microextraction (SPME) for the enantiomeric analysis of primary amphetamines by liquid chromatography has been investigated. Different derivatization/extraction strategies have been evaluated and compared using the chiral reagent o -phthaldialdehyde (OPA)– N -acetyl- l -cysteine (NAC) and fibres with a Carbowax-templated resin coating. Amphetamine, norephedrine and 3,4-methylenedioxyamphetamine (MDA) were used as model compounds. On the basis of the results obtained, a new method is presented based on the derivatization of the analytes in solution followed by SPME of the OPA–NAC derivatives formed. The proposed conditio…
Quantitative colorimetric analysis of some inorganic salts using digital photography
2011
An analytical imaging approach to the quantitation of dissolved chemical species absorbed in the visible spectral region is reported. The approach uses digital images of a series of standard solutions of the target substance and their processing with appropriate software to assign a numeric value to each standard in terms of color intensity. Such a value is directly proportional to the analyte concentration and allows the construction of a calibration graph. The results thus obtained are compared with those provided by the classical spectrophotometricmethod used to run calibration curves for colored substances. The chemical imaging technique is relative simple and affordable; in fact, it ca…
Real-time polarimetric biosensing using macroporous alumina membranes
2013
We report the first demonstration of real-time biosensing in free standing macroporous alumina membranes. The membranes with their 200 nm diameter pores are ideal candidates for biosensing applications where fast response times for small sample volumes are needed as they allow analytes to flow through the pores close to the bioreceptors immobilized on the pores walls. A bulk refractive index sensitivity of 5.2x10 -6 refractive index units was obtained from signal responses to different concentrations of NaCl solutions flowing through the pores. Finally, after functionalizing the alumina pore surfaces with an epoxysilane and then spotting it with β-Lactoglobulin protein, the interactions bet…
Optimisation of chromatographic resolution using objective functions including both time and spectral information.
2014
The optimisation of the resolution in high-performance liquid chromatography is traditionally performed attending only to the time information. However, even in the optimal conditions, some peak pairs may remain unresolved. Such incomplete resolution can be still accomplished by deconvolution, which can be carried out with more guarantees of success by including spectral information. In this work, two-way chromatographic objective functions (COFs) that incorporate both time and spectral information were tested, based on the peak purity (analyte peak fraction free of overlapping) and the multivariate selectivity (figure of merit derived from the net analyte signal) concepts. These COFs are s…
Target analysis and retrospective screening of mycotoxins and pharmacologically active substances in milk using an ultra-high-performance liquid chro…
2020
Milk is a nutritious food suitable for infants and adults, and it plays an important role in the human diet. However, it may also be a vehicle for food contaminants. In this report, we developed a method using ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap HRMS; Thermo Fisher Scientific, Waltham, MA) for simultaneous identification of target pharmacologically active substances and mycotoxins in milk. We also used the Q-Orbitrap operating in full scan mode to identify other possible drugs and microbial metabolites that occurred in samples. Fifty-six commercially available milk samples from the Italian market were analyze…
Science based calibration for the extraction of 'analyte-specific' HPLC-DAD chromatograms in environmental analysis
2010
Multivariate science based calibration (SBC) has been applied to the resolution of overlapped peaks in liquid chromatography with diode array detection (LC-DAD). Complex river water samples spiked with 11 pharmaceutical substances resulted in poorly resolved chromatograms containing additional peaks from interfering matrix compounds and a change in the background absorbance due to the mobile phase gradient. Applying the present multivariate approach it was possible to resolve all 11 analytes from overlapping peaks, obtaining linear calibration lines (R2 > 0.96). Recovery percentages on spiked samples ranged between 74.6 and 113.5%, which are quite satisfactory taking into account the low co…
Comparison between micellar liquid chromatography and capillary zone electrophoresis for the determination of hydrophobic basic drugs in pharmaceutic…
2007
[EN] The determination of highly hydrophobic basic compounds by means of conventional reversed-phase liquid chromatographic methods has several drawbacks. Owing to the characteristics of micellar liquid chromatography (MLC) and capillary electrophoresis (CE), these techniques could be advantageous alternatives to reversed-phase chromatographic methods for the determination of these kinds of compounds. The objective of this study was to develop and compare MLC and CE methods for the determination of antipsychotic basic drugs (amitryptiline, haloperidol, perphenazine and thioridazine) in pharmaceutical preparations. The chromatographic determination of the analytes was performed on a Kromasil…