Search results for "Sample preparation"
showing 10 items of 343 documents
Modelling phase transition kinetics of chenodeoxycholic acid with the Runge–Kutta method
2009
Abstract The phase transition kinetics of two chenodeoxycholic acid polymorphic modifications— form I (stable at high temperature), form III (stable at low temperature) and the amorphous phase has been examined under various conditions of temperature and relative humidity. Form III conversion to form I was examined at high temperature conditions and was found to be non-spontaneous, requiring seed crystals for initiation. The formation kinetic model of form I was created incorporating the three-dimensional seed crystal growth, the phase transition rate proportion to the surface area of form I crystals, and the influence of the amorphous phase surface area changes with an empirical stage poin…
Application potential of dummy molecularly imprinted polymers as solid-phase extraction sorbents for determination of low-mass polybrominated dipheny…
2019
Abstract Despite the introduction of restrictive regulations in the USA and the European Union, polybrominated diphenyl ethers (PBDEs) are still found in various types of environmental and biological samples at significant concentration levels. The presence of these persistent organic pollutants in the environment raises important issues because of their negative impact on immunological and neurological systems, and on the hormonal balances in living organisms. From the analytical point of view, the final determination of PBDEs would entail substantial challenges, because it would necessitate conducting the pre-concentration of analytes, or sample clean up. The aim of the present study is t…
Strategies for the rapid characterization of metals and organic pollutants in solid wastes and contaminated soils by using mass spectrometry
1998
Abstract Hyphenated techniques involving mass spectrometry (MS) such as ICP-MS, GC–MS and LC–MS are the most powerful tools for both qualitative and quantitative characterization of metals and organic pollutants in previously dissolved or extracted samples. However a considerable analytical effort is required in developing simple and general sample preparation strategies for the complete characterization of toxic substances in solid wastes and soils. This article gives a critical review of the state-of-the-art and future perspectives for rapid procedures to evaluate the pollution of soils and sediments, also considering new alternatives like flow injection analysis–MS and direct sampling MS.
FIA-AAS determination of salicylic acid by a solid-phase reactor of copper carbonate incorporated in polyester resin beads.
1994
Abstract The determination of salicylic acid was carried out by reaction of the drug with copper carbonate entrapped in a polymeric material in a solid-phase reactor; the released cupric ions were monitored by flame atomic absorption at 324.8 nm. The calibration graph is linear over the range 4.0–75 μg ml −1 of salicylic acid, with a relative standard deviation of less than 1.5% and a sample throughout of 257 h −1 . The influence of foreign compounds was studied and the method was applied to the determination of salicylic acid content in two different pharmaceutical formulations.
Analysis of toxic elements in plastic components for toys. Multi-elemental determination by x-ray fluorescence
1993
Abstract An x-ray fluorescence method is proposed for the multi-elemental determination of toxic elements in plastic articles for children, viz., Sb(III), Ba, Cd, Cr(III), Hg, Pb and As(III). Mineralization is achieved by using molten sodium hydroxide to decompose the organic matrix, with sodium nitrate as auxiliary oxidant. Stable solutions containing the chemical species for analysis are obtained. The species are separated from the solution by (co)precipitation, in a medium of NH+4-NH3 buffer (pH 8.5) with sodium diethyldithiocarbamate, sodium rhodizonate and Fe3+, which acts as a carrier. The precipitates deposited on filter-paper are placed in the x-ray spectrometer in fine layer morpho…
Evaluation of FASP, SP3, and iST Protocols for Proteomic Sample Preparation in the Low Microgram Range
2017
Efficient and reproducible sample preparation is a prerequisite for any robust and sensitive quantitative bottom-up proteomics workflow. Here, we performed an independent comparison between single-pot solid-phase-enhanced sample preparation (SP3), filter-aided sample preparation (FASP), and a commercial kit based on the in-StageTip (iST) method. We assessed their performance for the processing of proteomic samples in the low μg range using varying amounts of HeLa cell lysate (1-20 μg of total protein). All three workflows showed similar performances for 20 μg of starting material. When handling sample sizes below 10 μg, the number of identified proteins and peptides as well as the quantitat…
Sample Preparation for Mass-spectrometry-based Proteomics Analysis of Ocular Microvessels
2019
The use of isolated ocular blood vessels in vitro to decipher the pathophysiological state of the eye using advanced technological approaches has greatly expanded our understanding of certain diseases. Mass spectrometry (MS)-based proteomics has emerged as a powerful tool to unravel alterations in the molecular mechanisms and protein signaling pathways in the vascular beds in health and disease. However, sample preparation steps prior to MS analyses are crucial to obtain reproducible results and in-depth elucidation of the complex proteome. This is particularly important for preparation of ocular microvessels, where the amount of sample available for analyses is often limited and thus, pose…
Proteomics of CaCO3 biomineral-associated proteins: how to properly address their analysis.
2013
8 pages; International audience; In a recent editorial (Proc. Natl. Acad. Sci., 2013 110, E2144-E2146) and elsewhere, questions have been raised regarding the experimental practices in relation to the proteomic analysis of organic matrices associated to the biomineralized CaCO3 skeletons of metazoans such as molluscan shells and coral skeletons. Indeed, although the use of new high sensitivity MS technology potentially allows to identify a greater number of proteins, it is also equally (or even more) sensitive to contamination of residual proteins from soft tissues, which are in close contact with the biomineral. Based on our own past and present experimental know-how-observations that are …
Recent Advances in Affinity MOF-Based Sorbents with Sample Preparation Purposes
2020
This review summarizes the recent advances concerning metal–organic frameworks (MOFs) modified with several biomolecules (e.g., amino acids, nucleobases, proteins, antibodies, aptamers, etc.) as ligands to prepare affinity-based sorbents for application in the sample preparation field. The preparation and incorporation strategies of these MOF-based affinity materials were described. Additionally, the different types of ligands that can be employed for the synthesis of these biocomposites and their application as sorbents for the selective extraction of molecules and clean-up of complex real samples is reported. The most important features of the developed biocomposites will be discussed thr…
Matrix solid-phase dispersion microextraction and determination by high-performance liquid chromatography with UV detection of pesticide residues in …
1999
A multiresidue method based on matrix solid-phase dispersion (MSPD) microextraction was studied to determine the carbamate, benfuracarb, and urea insecticides, diflubenzuron, flufenoxuron hexaflumuron and hexythiazox, used in control of citrus pests. Optimisation of different parameters, such as the type of solid support for matrix dispersion, elution solvents and the clean-up step were carried out. The method used 0.5 g of orange sample, C8 bonded silica as MSPD sorbent and dichloromethane as eluting solvent. Recoveries, at spiked concentrations below the maximum residue levels established by Spanish Government, were between 74 and 84% with relative standard deviations ranging from 2 to 4%…