Search results for "Analytical"
showing 10 items of 9586 documents
Headspace-Liquid Phase Microextraction for Attenuated Total Reflection Infrared Determination of Volatile Organic Compounds at Trace Levels
2010
A combination of headspace (HS) sampling and liquid phase microextraction (LPME) has been successfully developed to solve sensitivity problems in attenuated total reflection (ATR) infrared determination of volatile organic compounds (VOCs). The HS sampling facilitates the selective extraction of the target volatile analytes from the sample matrix, while the liquid phase microextraction allows their preconcentration prior to infrared analysis. The direct determination of extracted analytes in the acceptor solvent provides high preconcentration factors of the order of 200 with a reduced consumption of organic solvents and a minimum generation of wastes, being thus the developed methodology a …
Reversed-phase liquid chromatography without organic solvent for determination of tricyclic antidepressants
2012
The chromatographic behavior of seven tricyclic antidepressants (amitryptiline, clomipramine, doxepin, imipramine, maprotiline, nortryptiline, and trimipramine) was examined with micellar mobile phases containing the nonionic surfactant Brij-35. Acetonitrile-water mixtures were also used for comparison purposes. Tricyclic antidepressants are moderately polar basic drugs, which are positively charged in the usual working pH. This gives rise to a strong association with the alkyl chains and residual ionized silanols in silica-based stationary phases, which is translated in a high consumption of organic solvent to get appropriate retention times. Brij-35 modifies the surface of the stationary …
Simultaneous gas chromatographic determination of aliphatic C2−C20 n-carboxylic acids and their methyl esters using SE-30 and OV-351 quartz capillary…
1983
Simultaneous determination of aliphatic C2−C20 carboxylic acids and their methyl esters was carried out using SE-30 and OV-351 quartz capillary columns with temperature programming. Complete resolution of all 36 components was achieved. On SE-30 the methyl ester and the corresponding free acid are eluted in turn, whereas on OV-351 acetic acid eluted after methyl octanoate, after which the Cn methyl ester and Cn-6 carboxylic acid (n>9) are eluted one after the other. A non-polar SE-30 column is better for long-chain acids giving sharp peaks without tailing, the analysis time of the mixture being less than 16 minutes. The weight response correction factors for compounds under optimum operatin…
Selective extraction of small proteins from biological samples using a novel restricted access column with cation exchange properties
2000
The determination of proteins utilising a polymer-based restricted access suppor material with ion exchange properties (IERAM) is outlined. Solid phase extraction coupled on-line with a mincrobore reversed phase HPLC system for the quantitation of small marker proteins is demonstrated. The cation-exchange restricted access packings were characterised with respect to their adsorption and desorption kinetics. The IERAM material was also investigated by capacity, selectivity, and biocompatibility determinations when applied to the quantification of small molecular weight proteins such as cytochrome C, Lysozyme, Ribonuclease A, Myoglobin, Insulin, human serum albumin, and a Tryptic inhibitor.
Continuous fractionation and solution properties of PIB. I. Search for the best mixed solvent and first results of the continuous polymer fractionati…
1987
To adopt a recently developed method for large scale fractionation (CPF = continuous polymer fractionation, a special kind of counter current extraction) to polyisobutylene (PIB), a systematic search for the best mixed solvent was performed. For this purpose, the essential parts of the phase diagrams solvent/nonsolvent/PIB were determined for 21 mixed solvents by cloud-point measurements; with eight systems of special interest, the molecular weight distributions of the polymers contained in the coexisting phases were also studied. On the basis of these experiments and of considerations concerning additional criteria for the performance of the continuous counter current extraction, the mixed…
Retention behaviour of paracelsin peptides on reversed-phase silicas with varying n-alkyl chain length and ligand density.
1989
As part of further investigations on the characterization of the ligand-induced conformational stabilization of peptides, two series of n-alkyldimethylsilyl bonded silicas have been prepared. In series A the n-alkyl chain length, n, of the bonded phase was varied between 1 and 20 carbon atoms at a constant ligand density. In series B the ligand density, alpha exp, was gradually changed from 0 to 4.1 mumol/m2 on a C1, C4, C6, C8 and C18 bonded phase. The retention behaviour of four peptides of the paracelsin family were examined under isocratic conditions, using a ternary mobile phase of water-methanol-acetonitrile (22:39:39, v/v/v). Plots of k' versus n showed pronounced maxima between n = …
Imprinted chiral stationary phases in high-performance liquid chromatography
2001
Polymers imprinted with chiral templates offer a new generation of tailor-made chiral stationary phases (CSPs) with predictable selectivities. This review summarizes the present state of the art of molecular imprinting to generate tailor-made CSPs and provides an overview of the main factors involved in the manufacturing process that are crucial to the chromatographic performance of the phases.
Detection of poly(methylmethacrylate) wear particles in capsule tissue surrounding endoprotheses by pyrolysis gas chromatography
1982
Pyrolysis gas chromatography (PGC) is used to detect polymer wear particles in capsule tissue surrounding endoprotheses implanted with poly(methylmethacrylate) as bone cement. The method allows the detection of the polymer incorporated in tissue even in the range of 1 weight%.
Separation studies of amino acids, proteins and enzymes on bonded 1,2-dihydroxy-, 1,2-hydroxylamino-and amino silica packings
1979
1,2-dihydroxy-3-propoxypropyl (HPPS), 1-amino-2-hydroxy-3-propoxypropyl (AHPS) and 1-aminoethyl-3-aminopropyl (AEAPS) silica were synthesized by means of both a surface modification procedure (I) and a bulk modification procedure (II). Method (I) gave a surface concentration, α, of functional groups of 2–3 μmole/m2, whereas method (II) gave values up to 5 μmole/m2. Retention times, peak asymmetries and plate heights of thiamine and ascorbic acid eluted with aqueous buffer solutions ranging from pH 5.3 to 9.2 gave only a±5% variation over periods of 12 hours and more. The recoveries of selected enzymes and proteines examined under static and dynamic conditions were between 60% and 100% depen…
Development of a semiautomated procedure for the synthesis and evaluation of molecularly imprinted polymers applied to the search for functional mono…
2001
Abstract A previously described scaled-down version of the established monolith procedure, where molecularly imprinted polymers (MIPs) are prepared on the bottom surface of chromatographic vials [Anal. Chem. 71 (1999) 2092] has been here further optimised with respect to its full automation. The protocol results in savings of time and reagents compared to the monolith procedure, allowing ca. 60 polymers (∼50 mg each) to be synthesised in parallel. Both blank and imprinted polymers are then evaluated in situ by equilibrium batch rebinding tests. Each step in the synthesis and evaluation was considered with the aim of achieving an automated method with wide applicability with regards to templ…