Search results for "Extraction"

Determination of theophylline and paraxanthine in urine samples by liquid chromatography using the H-point standard additions method

1992

Abstract The simultaneous determination of theophylline and paraxanthine in urine samples by the H-point standard additions method (HPSAM) is described. Samples are extracted with C 18 solid-phase extraction cartridges and chromatographed using a Hypersil C 18 -ODS column and a mobile phase consisting of acetonirile-phosphate buffer in the gradient elution mode. Under these conditions theophylline and paraxanthine are eluted with short retention times. Although their chromatographic peaks are overlapped and their spectra are very similar, the H-point standard additions method provides excellent results in the determination of both xanthines at therapeutic levels.

Solid-phase extraction of quaternary ammonium herbicides

2000

This paper highlights recent advances in the solid-phase extraction (SPE) of quaternary ammonium herbicides in water, soil, plant and biological samples. After a brief introduction summarizing the properties of quaternary ammonium herbicides and the difficulties involved in measuring them, attention is paid primarily to solid supports used for isolation and concentration, pre-treatments required for the different matrices, and eluents applied for quantitative desorption of these analytes. The determination techniques used after SPE and applications of the proposed SPE methodology are also briefly discussed.

High-pressure solubility data of system ethanol (1)+catechin (2)+CO2 (3)

2001

Abstract Supercritical fluid extraction posses several advantages over traditional liquid–solvent-based extraction methods including improved selectivity, expeditiousness, automation and environmental safety. Fluid phase equilibrium data is essential for study the viability of supercritical extraction and the design of the extraction columns often used for this type of separations. During the past few years it has been demonstrated that phenolic compounds, such catechins and procyanidins from seeds, contribute to both the flavour properties and the pharmacological effects of wine. The extraction of catechin using supercritical CO2 is not possible, it only extracts traces of product, probabl…

High-pressure solubility data of the system resveratrol (3)+ethanol (2)+CO2 (1)

2001

Abstract Supercritical fluid extraction possesses several advantages over traditional liquid-solvent-based extraction methods, including improved selectivity, expeditiousness, automation and environmental safety. Fluid-phase equilibrium data are essential for studying the viability of supercritical extraction and the design of the extraction columns often used for this type of separation. Resveratrol has been correlated with serum lipid reduction and inhibition of platelet aggregation, and its cancer chemopreventive activity has recently been reported. The extraction of resveratrol using supercritical CO 2 is not possible; it only extracts traces of product, probably due to its polar nature…

Chromium(VI) oxide oxidation of non-ethoxylated and ethoxylated alcohols for determination by electrospray ionization mass spectrometry

2010

A new derivatization procedure to increase the sensitivity of electrospray ionization mass spectrometry (ESI-MS) to non-ethoxylated and ethoxylated alcohols was investigated. The analytes were oxidized with chromium(VI) oxide and the resulting carboxylic and ethoxy-carboxylic acids were isolated by extraction with ethyl acetate; the extracts were alkalinized and infused into the ESI-MS system working in the negative-ion mode. The yields of the combined oxidation-extraction were ca. 100% for non-ethoxylated fatty alcohols dissolved in acetone and they decreased moderately in samples containing increasing amounts of water (e.g., a 75% yield was obtained with 50% water). Ethoxylated alcohols w…

Analysis of neuropeptide Y and its metabolites by high-performance liquid chromatography-electrospray ionization mass spectrometry and integrated sam…

2000

A novel restricted access cation exchanger with sulphonic acid groups at the internal surface was proven to be highly suitable in the sample clean up of peptides on-line coupled to HPLC-electrospray ionization (ESI)-MS. Neuropeptide Y (NPY) and several of its fragments in plasma were subjected to the sample clean-up procedure. The peptides were eluted by a step gradient from the restricted access column, applying 10 mM phosphate buffer pH 3.5 from 5 to 20% (v/v) of acetonitrile with 1 M NaCl and transferred to a Micra ODS II column (33x4.6 mm). The separation of the peptides and their fragments was performed by a linear gradient from 20 to 60% (v/v) acetonitrile in water with 0.1% formic ac…

Determination of pyrethroid insecticide residues in vegetable oils by using combined solid-phases extraction and tandem mass spectrometry detection

2005

Abstract A methodology has been developed for the determination of pyrethroid insecticide residues in vegetable oils, based in a solid-phase extraction (SPE) with combined solid supports phases. Several solid phases such as florisil, alumina, C18 and graphitized carbon black were tested in order to minimize fat residues, being a combination of treated alumina and C18 which provided the best results. Oil samples were partitioned with acetonitrile–hexane (1:1) and then eluted through a combined column packed with deactivated basic-alumina and C18, employing the acetonitrile extract as elution solvent. Gas chromatography tandem mass spectrometry was used for determination. Tetramethrin, Bifent…

Free fatty acids and other volatile compounds for the characterisation of “Vastedda della valle del Belìce” cheese Acidos grasos libres y otros const…

2010

The analysis of the volatile constituents of “Vastedda della valle del Belice”, a typical Sicilian pasta filata cheese, was performed using solid phase microextraction and high-resolution gas chromatography/mass spectrometry. The research aimed to verify if the volatile fraction, determinant for cheese flavor, differs among producers and/or production seasons. The samples were provided by four producers from the area of the Protected Designation of Origin (PDO) production, during two different seasons of production. A total of 42 volatile components were identified: the main components were found to be butanoic, hexanoic, octanoic, and decanoic acid. Free fatty acids were quantified using t…

Multi-mycotoxin analysis in North African semolina samples using a modified QuEChERS-based extraction procedure and HPLC–MS/MS

2014

Sulphonic acid strong cation-exchange restricted access columns in sample cleanup for profiling of endogeneous peptides in multidimensional liquid ch…

2006

Abstract In this work, the pore structural parameters and size exclusion properties of LiChrospher strong cation-exchange and reverse phase restricted access materials (RAM) are analysed. The molecular weight size exclusion limit for polystyrenes was found to be about 17.7 kDa, while for standard proteins, the molecular weight size exclusion limit was higher, at approximately 25 kDa. The average pore diameter on a volume basis calculated from the pore network model changes from 8.5 nm (native LiChrospher) to 8.6 nm (diol derivative) to 8.2 nm (sulphonic acid derivative) to 6.9 nm ( n -octadecyl derivative). Additional characterisations were performed on restricted access materials with nitr…