Search results for "Sample preparation"
showing 10 items of 343 documents
The development and validation of a rapid method for the determination of antimicrobial agent residues in milk and meat using ultra performance liqui…
2014
Abstract A new multi-class method has been developed for the identification and quantification of the residues of 26 antibiotics from different classes (sulfonamides, macrolides, tetracyclines, penicillins, and quinolones) in milk and meat by ultra performance liquid chromatography coupled to hybrid quadrupole – high resolution Orbitrap mass spectrometry (UPLC–qOrbitrap). The sample preparation included extraction of two analytical portions with acetonitrile and 5% trichloroacetic acid, respectively, followed by centrifugation and filtration. The method was validated over three days at 50% of MRL (maximum residue limit) set in the European Union. Experiments on spiked meat and milk samples …
Determination of the mineral composition of foods by infrared spectroscopy: a review of a green alternative.
2014
The determination of mineral composition of foods involves, in most cases, the use of long and tedious sample preparation, which consumes acids and reagents and sometimes requires the use of expensive instrumentation. This is the main reason for the search for direct analytical procedures, based on the use of infrared sample spectra and chemometrics, to model the signals in order to determine the presence of essential and trace toxic elements in foods. The state-of-the-art of the research in this field has been established in the present review article from the critical evaluation of articles available in the literature. Chemometric methods employed and their validation, together with a dis…
Characterization of isomeric 1,2,4-oxadiazolyl-N-methylpyridinium salts by electrospray ionization tandem mass spectrometry.
2007
The mass spectrometric behavior of 1,2,4-oxadiazolyl- N-methylpyridinium salts has been investigated. These substances are of current interest as perspective ionic liquids, compounds used as green solvents for synthesis, and for their catalytic properties. The studies have been developed through electrospray ionization tandem mass spectrometry (ESI-MS/MS) experiments. The obtained results demonstrate a ready distinction between the two isomeric classes, 3- N-methylpyridinium- and 5- N-methylpyridinium-1,2,4-oxadiazoles, is possible through ESI-MS/MS experiments. A deeper investigation on the principal fragmentation pathways of characteristic ions has been also developed.
Investigation of the phase transitions occurring during and after the dehydration of xylazine hydrochloride monohydrate.
2014
This paper reports an investigation of a complex solid state phase transition where two inter-converting polymorphs (X and A) of the pharmaceutical molecule xylazine hydrochloride formed and transformed during and after the dehydration of its monohydrate (H). The crystal structures of all three forms were compared. During the investigation of this solid state phase transition it was determined that the dehydration of H produced either a pure X form, or a mixture of the X and A forms. The phase composition depended on the sample preparation procedure and the experimental conditions. It was found that grinding of the hydrate enhanced the formation of polymorph X as a product of dehydration, w…
Recent advances in aptamer-based miniaturized extraction approaches in food analysis
2021
Abstract Sample preparation is a relevant step in food analysis to achieve adequate extraction and preconcentration of target analytes before their introduction in the analytical system. Current trends in sample preparation involve moving towards miniaturized extraction devices combined with advanced affinity-based sorbents. Within affinity-based materials, aptamer-based ones have attracted much attention due to their excellent molecular recognition properties, high stability, and the possibility of immobilization onto the surface of different supporting materials, such as nanoparticles, monolithic stationary phases, etc. This review gives an overview of the literature published regarding a…
Monolithic silica columns of various format in automated sample clean-up/multidimensional liquid chromatography/mass spectrometry for peptidomics.
2007
The following particulate and monolithic silica columns were implemented in a fully automated and flexible multidimensional LC/MS system with integrated sample clean-up, to perform the analysis of endogeneous peptides from filtered urine and plasma samples: restricted access sulphonic acid strong cation-exchanger (RAM-SCX) for sample clean-up, RP 18 Chromolith guard columns as trap columns and 100 microm I.D. monolithic RP 18 fused silica capillary columns as last LC dimension. The results show sufficient overall system reproducibility and repeatability. Implementation of monolithic silica columns added an additional flexibility with respect to flow rate variation and adjustment due to the …
Combination of mid- and near-infrared spectroscopy for the determination of the quality properties of beers
2006
Abstract The combination of infrared (MIR) and near-infrared (NIR) spectroscopy has been employed for the determination of important quality parameters of beers, such as original and real extract and alcohol content. A population of 43 samples obtained from the Spanish market and including different types of beer, was evaluated. For each technique, spectra were obtained in triplicate. In the case of NIR a 1 mm pathlength quartz flow cell was used, whereas attenuated total reflectance measurements were used in MIR. Cluster hierarchical analysis was employed to select calibration and validation data sets. The calibration set was composed of 15 samples, thus leaving 28 for validation. A critic…
Influence of sample preparation on analytical results: drug analysis [GC/MS] on hair snippets versus hair powder using various extraction methods
1997
The comparison of aqueous extraction methods and hair extraction by organic solvents performed on hair powder as well as on hair snippets of the same sample revealed different qualities of the procedures. Qualitative and quantitative results by the same derivatization step and GC/MS detection demonstrated, that the risk of missing a drug substance is higher using hair snippets than after drug extraction on pulverised hair. Drug recovery for opiates, cocaine and benzoylecgonine from hair was found to be best in aqueous solvents or in methanol extracts. The results are discussed under the aspects of solid-phase extraction, the hair sample representing an inhomogenous material. The localisatio…
Laser spectroscopy of radioactive isotopes
1987
The experimental conditions for laser spectroscopy of shortlived isotopes is discussed with respect to nuclear lifetime, reaction rates and samples preparation by on-line mass-separator techniques. The method of collinear laser spectroscopy is presented with results for medium mass elements near the closed proton shell Z=50. An interpretation of magnetic moments, spectroscopic quadrupole moments and the parabolic shape of the isotope shift in this region of nuclei is given.
Simulation studies of the laser ablation ion source at the SHIPTRAP setup
2020
Hyperfine interactions 241(1), 46 (2020). doi:10.1007/s10751-020-01708-0