Search results for "analytical"
showing 10 items of 9586 documents
Origin of peak asymmetry and the effect of temperature on solute retention in enantiomer separations on imprinted chiral stationary phases
1995
Abstract In enantiomer separations of d - and l -phenylalanine anlilide ( d,l -PA) on l -PA-imprinted chiral stationary phases (CSPs), the use of an aqueous buffer-organic solvent mixture as mobile phase resulted in improved column efficiency compared with what has previously been observed using mobile phases containing acetic acid as modifier. The dependence of the chromatographic parameters on flow-rate and sample load was studied. A strong dependence of the asymmetry factor ( A s ) of the l -form on sample load and a weak dependence on flow-rate indicate that the non-linear adsorption isotherm is the main reason for the broad peaks observed in this system. Depending on the method used fo…
Characterisation of humic substances by acid catalysed transesterification
2002
Abstract The chemical composition of low molecular weight moieties linked to the core structures of humic substances (HS) are of substantial importance for the understanding of the chemical structures and mode of interactions of HS with other substances in the environment. In this study a novel approach to characterise certain low molecular weight compounds bound to HS is suggested. The method includes transesterification (TE) of ester and amide bound structures, and esterification (E) of free carboxylic groups using acid catalysed methanolysis followed by gas chromatography (GC)–mass spectrometry (MS) and GC-FID analysis. Methanolysis of five HS of different origin, demonstrated the presen…
Preparation of nanostructures composed of dextran sulfate/ruthenium nanoparticles and their interaction with phospholipid monolayers at a liquid–liqu…
2007
Abstract Nanostructures composed of dextran sulfate (DS)/ruthenium (Ru) nanoparticles (NPs) adsorbed on phospholipid monolayers at a liquid–liquid interface were prepared and characterized electrochemically in relation to their potential use in drug delivery systems. First, positively charged Ru NPs were prepared, and then negatively charged DS was adsorbed on the surface of the NPs, thus forming well-defined and organized structures, as observed under the transmission electron microscope, which are referred to composite nanoclusters. The lipid monolayers were formed by depositing either 1-palmitoyl-2-oleoyl- sn -glycero-3-phosphatidylcholine or 1-palmitoyl-2-oleoyl- sn -glycero-3-phospho- …
Use of SPME extraction to determine organophosphorus pesticides adsorption phenomena in water and soil matrices
2005
Solid-phase micro extraction (SPME) coupled with GC enables rapid and simple analysis of organophosphorus pesticides in a range of complex matrices. Investigations were made into the extraction efficiencies from water of six organophosphorus insecticides (methamidophos, omethoate, dimethoate, parathion methyl, malathion, and parathion ethyl) showing a wide range of polarities. Three SPME fibres coated with different stationary phases, polydimethylsiloxane, polyacrylate, and carbowax-divinylbenzene (CW-DVB), were investigated. Water was spiked with the pesticides at concentrations from 1 to 0.01 µg mL-1, and the solutions used for optimization of the procedure. The CW-DVB fibre, with a 65 µm…
Novel porous carbon packings in reversed-phase high-performance liquid chromatography
1980
Abstract Porous carbon packings of particle size 5–20 μm were prepared by calcination of purified active carbons and cokes having narrow size ranges. Highly efficient columns packed with 10-μm particles were obtained by means of the high-viscosity slurry technique, and exhibited about 3000 theoretical plates at 100 mm length and optimal eluent flow-rate. The loading of columns, θ0.1, was determined to be 25–50 μg of solute per gram of packing. Eluotropic series of solvents were found to be similar to those on pyrocarbon-modified carbons and silicas. The log k′ values for homologous compounds increased linearly with the hydrocarbonaceous surface area at constant eluent composition. Studies w…
FIA-fluorimetric determination of adrenaline in pharmaceutical formulations by oxidation with molecular oxygen
1998
The fluorimetric determination of adrenaline is carried out in a continuous-flow assembly and by means of the molecular dissolved oxygen. The sample solution merges with an NaOH stream, then the resulting mixture is heated at 73 °C and led to the flow-cell of the fluorimeter. The flow-assembly is very simple and the procedure is quick (107 samples h−1) reproducible (R.S.D. 0.6%), selective and suitable to be applied to determination of adrenaline in formulations. Calibrations graph are linear over the ranges 0.05–15 and 20–40 mgl−1.
Gas assisted mechanical expression (GAME) for the selective recovery of lipophilic and hydrophilic compounds from olive kernel
2017
Abstract This work is devoted to valorize olive kernel; a by-product produced during olive oil extraction process. For this purpose, aqueous liquid solid extraction (LSE), mechanical expression (ME), supercritical CO2 (SC-CO2) and gas assisted mechanical expression (GAME), processes were compared when applied separately or consequently (ME + GAME), in terms of total phenolic compound (TPC) and oil recovery yields. Results showed that although the high extraction yields of TPC using LSE (61.4 ± 1.3%), the extraction process is economically not viable. However, it was demonstrated that applying ME (1 h at 30 MPa) followed by GAME (1 h at 30 MPa ME and 10 MPa SC-CO2 pressures) allowed recoveri…
Screening and authentication of herbal formulations based on microextraction-assisted voltammetry of microparticles
2015
A simple solid state electrochemical methodology for screening and authentication of herbal formulations is described. The proposed method is based on the recording of the voltammetric response, in contact with aqueous buffers, of microparticulate films of antioxidant compounds resulting from micro-extraction of dried herbal samples with ethanol or acetone. The obtained voltammetric responses led us to differentiate between diverse active components upon application of bivariate and multivariate chemometric techniques. Resolution of herbal preparations containing two or more components is possible when well-separated voltammetric signals are recorded. In favorable cases, such characteristic…
Simultaneous Determination of Adrenaline and Noradrenaline by First Derivative Spectrophotometry in a Fia Assembly
1996
Abstract This article deals with the design of an unsegmented-flow injection manifold for the simultaneous determination of adrenaline and noradrenaline two structurally related compounds with overlapping spectra. An FIA manifold is proposed for the simultaneous determination in which the sample solution is directly injected into a carrier-reagent stream of aqueous NaOH. The selected wavelengths (first derivative) were 394 and 342 nm, for noradrenaline and adrenaline, respectively with an integration time of 0.4 s. The calibration graphs are linear over the range 2.0–30 ppm for both drugs. The method is applied to different synthetic mixtures of both drugs.
The use of utraviolet-visible spectrophotometry in the determination of average properties of nonylphenol ethylene oxide condensates
1983
Ultraviolet spectrophotometry is usd in the determination of average molecular weight (M), average degree of polymerization (X), the hydrophilic-lipophilic balance (HLB) and ethylene oxide percentage of nonylphenol ethylene oxide condensates. The method is based on determination of the absorptivity a, expressed in g lt-1 cm−1, from the absorbances measured at 275 nm for a series of dilutions of an aqeuous ethanolic solution (60:40, v/v/) of a given product, followed by numerical interpolation of this value in the expression a = f(HLB), log a = f(log M), and log a = f(log X). These expressions are obtained from reference samples or samples previously analyzed. The proposed method gives relat…