Search results for "Solid"

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.

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…

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…

Pesticides (New Generation) and Related Compounds, Analysis of

2017

Miscellaneous pesticides and related compounds comprise substances that can neither be included in the classical chemical category of pesticides nor classified by their mode of action. They are a heterogeneous group of substances, the most representative of which are macrocyclic lactones, chloronicotinyls, tetranortriterpenoids, ammonium quaternary salts, dinitroanilines, acetamides, oximes, triazoles, and pyridine-based molecules. The pesticides covered in this article have hardly changed in the last years. However, their analytical determination has undergone significant improvements. This article provides a well-defined and critical compilation of the sample treatment and clean-up proced…

New insights on the thermal analysis of low moisture composite foods.

2014

Abstract Low moisture baked products were investigated with a view to characterising the effect of both formulation and humidity on their physical stability. At the end of the baking process, the samples were in the amorphous state as a result of starch gelatinization and sugar melting. Their thermal properties were analyzed with differential scanning calorimetry and their glass transitions were studied. The DSC thermograms were thoroughly studied through a Gaussian deconvolution of the first derivative of their heat flow. This approach evidenced a multiple phase behavior with different glass transitions in composite systems. They were associated with either a polymer-rich phase and/or a pl…

HERBICIDES | Solid-Phase Extraction

2000

Pleurotus ostreatus volatile aroma compounds identified from fruit-body and from mycelium grown in submerged and solid-state cultures

2003

Comparative analyses of volatile aroma compounds of the Pleurotus ostreatus JMO.95 fruit-body and its corresponding mycelium grown in liquid, on agar surface, or on solid support cultures have been carried out by dynamic headspace concentration using GC/MS and GC/sniffing. The aroma of the fruit-body was due essentially to the presence of octan-3-one and, in a lesser extent, to the presence of octan-3-ol. Other compounds, such as oct-l-en-3-ol, oct-l-en, 2-methylbutanol and a-pinene were also present in low concentrations. The comparison of the aromatic spectra of the fruit-body with the aromatic spectra of mycelia obtained under different culture conditions indicated that the main aromatic…

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…