Search results for "Analytical"

Separation of unmodified α-amino acid enantiomers by reverse phase HPLC

1980

A novel chiral phase system is presented for the resolution of unmodified α-amino acid racemates which is composed of a reverse phase packing coated with N-alkyl-L-hydroxyproline (where alkyl is n-C7H15-, n-C10H21- and n-C16H33-) and a hydro-organic eluent containing copper(II)acetate. The factors controlling retention and enantioselectivity such as concentration of Cu(II)ion and pH of the eluent, addition of NH4Ac to the eluent, type and content of organic solvent of hydro-organic eluent and column temperature were examined. The extremely high enantioselectivity observed (α up to 16) is assumed to be caused by a three site sorbate-sorbent interaction involving bidentate coordination of two…

Correlation between hydrophobicity of amino acids and retention data in reversed-phase liquid chromatography with micellar eluents

1995

Hydrophobic character is usually expressed in terms of the partition coefficient in 1-octanol-water (log PO/W). However, measurement of this coefficient is often problematic. Retention in micellar liquid chromatography is mainly due to hydrophobic interactions and can also be used as an index of hydrophobicity. A hydrophobicity scale was established with retention data foro-phthalaldehyde (OPA)-N-acetyl-L-cysteine (NAC) amino acid derivatives, using the glycine derivative as reference. Since the OPA-NAC derivatives only differ in the nature of R1 in the amino acid (R1CH(COOH)NH2), in the absence of electrostatic interactions the hydrophobic character of the substituent was responsible for r…

Gas-liquid chromatography and lipophilicity of esters of benzoic acids

1987

Abstract The use of gas-liquid chromatographic (GLC) retention indices for the determination of lipophilicity was studied for a series of alkyl and arylalkyl esters of substituted benzoic acids. The regression relationships between the logarithms of the partition coefficients and the retention characteristics measured on two cpillary columns, SE-30 and OV-351, were evaluated. The behaviour of arylalkyl esters and of alkyl esters cannot be expressed in terms of a single regression equation. This is probably a consequence of the effect of the intramolecular hydrophobic interaction upon the retention of arylalkyl esters under GLC conditions. An analysis of the isokinetic relationships revealed…

Polymer-coated reversed-phase packings with controlled hydrophobic properties

1992

Abstract We have designed and synthesized novel reversed-phase packings of non-porous and porous polymethacrylate-coated silicas. By varying the hydrophobicity of the polymer coating, selective unfolding of polypeptides may be achieved, thus enabling manipulation of the chromatographic profile. This study characterizes these packings through their employment for separations of model synthetic peptides of defined secondary, tertiary and quaternary structure. Thus, the packings were applied to the reversed-phase separation α-helical amphipathic and non-amphipathic peptides of the same amino acid composition but different sequences. In addition, selective unfolding of model to-stranded α-helic…

Chromatographic quantitation of the hydrophobicity of ionic compounds by the use of micellar mobile phases

1998

Abstract Many biologically active compounds of interest in structure–activity relationships are ionic at physiological pH. However, ionic organic compounds are only weakly or not retained in conventional RPLC which impedes the chromatographic estimation of their hydrophobicity and the development of quantitative retention–activity relationship studies. The use of micellar mobile phases allows the retention of ionic compounds. Hydrophobic and electrostatic forces govern the retention of ionic compounds in micellar liquid chromatography. In this paper three different retention models log k–log P for ionic compounds are tested (P=partition coefficient). The retention model (log k=a log P+bα+c)…

Effect of the hydrophobic spacer in bonded [Cu(l-hydroxyprolyl)alkyl]+ silicas on retention and enantioselectivity of α-amino acids in high-performan…

1983

Abstract The following chiral ligands were bonded to silica: [Cu( l -hydroxyprolyl)methyl) + on LiChrosorb Si 60 (1), [Cu( l -hydroxyprolyl)methyl] + on LiChrosorb Si 100 (2) and [Cu( l -hydroxyprolyl) n -octyl] + on LiChrosorb Si 100 (3). The packings contained residual iodomethyl- and ω-iodooctyl groups at the surface. Studies on packing 1 and 2 under comparable conditions in eluents containing 10 -4 M copper acetate showed a higher retention on 1 than on 2 but a much better enantioselectivity in the latter case. The retention of enantiomers on all packings examined was found to be governed by the eluent pH and methanol content as well as by the concentration of ammonium acetate. The vari…

New reagent for the detection of sesquiterpene lactones by thin-layer chromatography.

1984

Packings of an unidimensional regular pore structure as model packings in size-exclusion and inverse size-exclusion chromatography

1996

Using porous aluminas and aluminosilicates with a regular and well-defined pore structure an attempt was made to correlate the SEC data of polystyrenes with established theoretical models. The pore structure of the two types of packings was extensively characterized by means of transmission and scanning electron microscopy, nitrogen sorption and mercury porosimetry. The SEC distribution coefficients measured experimentally were correlated with the distribution coefficients calculated from the theoretical models for flexible polymers. A good correlation was observed for the packing of the simplest pore morphology, but remarkable deviations appeared for the materials with a more complex pore …

Application of molecularly imprinted polymers in supercritical fluid chromatography

2000

Molecularly imprinted polymers (MIPs), for the templates free base racemic propranolol and the L-enantiomer of phenylalanine anilide (L-PA), were investigated as stationary phases in supercritical fluid chromatography (SFC). Large retention differences were observed on the propranolol MIP for both the template molecule and the structural analogue metoprolol compared to that observed on the corresponding blank polymer. Mobile phase composition and solute concentration were found to affect this retention behaviour. The phenylalanine anilide MIP (L-PA MIP) was found to be enantioselective in SFC with stronger retention observed for the template enantiomer. Throughout the study, characteristic …

Characterization of commercial synthetic resins by pyrolysis-gas chromatography/mass spectrometry: application to modern art and conservation.

2009

To characterize a set of synthetic resins, a methodology by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) has been developed. The studied reference materials were commercial versions of a wide range of synthetic resins. For each polymer, the pyrolytic and chromatographic conditions were optimized to adequately resolve the fragment mixture in a short time. The proposed analytical method does not require previous treatment of the sample, and due to its high sensitivity, only a small sample quantity in the microgram range can be used. The pyrolysis temperature was found to have little effect on the obtained pyrograms. The summarized data set for the individual polymer materials, es…