Search results for "Sample"

Rapid method for analysis of nicotine and nicotine-related substances in chewing gum formulations

1998

Abstract Based on environmental requirements and demands for a high throughput a rapid method for the analysis of nicotine and nicotine-related substances in chewing gum formulations was developed. The method is based on sample preparation through liquid–liquid extraction followed by reversed-phase HPLC using gradient elution. It allowed up to nine analytes to be determined within 15 min, including the sample preparation, and was considered as accurate and robust.

Extraktionschromatographische trennung der freien porphyrine auf tri-n-butylphosphat-s?ulen im pH-gradienten

1969

Abstract The method described allows the separation of the free porphyrins on a tri-n-butyl phosphate (TBP) column by elution with a pH gradient. The prophyrins are eluted from the column at discrete pH values (xD) according to the number of carboxyl groups in the side chains. Separation of isomers could not be observed under the conditions used. The xD values indicate the centre of the pH-interval, in which the dissociation of the carboxyl groups occurs. This finding could be confirmed by spectro-photometric measurements. By combining the method proposed with the method of separation by extraction chromatography in the TBP/IN HCl partition system and the thin-layer technique in the 2,6-lut…

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.

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…

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…

An automated on-line multidimensional HPLC system for protein and peptide mapping with integrated sample preparation.

2002

A comprehensive on-line two-dimensional 2D-HPLC system with integrated sample preparation was developed for the analysis of proteins and peptides with a molecular weight below 20 kDa. The system setup provided fast separations and high resolving power and is considered to be a complementary technique to 2D gel electrophoresis in proteomics. The on-line system reproducibly resolved approximately 1000 peaks within the total analysis time of 96 min and avoided sample losses by off-line sample handling. The low-molecular-weight target analytes were separated from the matrix using novel silica-based restricted access materials (RAM) with ion exchange functionalities. The size-selective sample fr…

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…

Determination of several aminoglycoside and macrolide antibiotics in animal tissues by liquid chromatography-electrospray ionization-tandem mass spec…

2008

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…

Miniature diamond-anvil cells for FTIR-microspectroscopy of small quantities of biosamples.

2018

Fourier transform infrared (FTIR) spectroscopy techniques and data analyses have become widely available, are easy to use, and are convenient for studies of various biosamples, especially in biomedical science. Yet, cultivation of cells and purification of cell components are costly, often methodically challenging, and time and labor consuming. Therefore, reduction of the sample amount is of high value. Here we propose a novel method for the analysis of small quantities of biosamples by FTIR-microscopy of dry films using a diamond-anvil cell (DAC). This approach allows us to decrease the sample volume at least a hundred times compared to that for a high-throughput screening device (HTS-XT, …