0000000000704098

AUTHOR

J. M. Sanchis Mallols

Quantitative retention—structure and retention—activity relationship studies of ionic and non-ionic catecholamines by micellar liquid chromatography

When ionic surfactants are used as mobile phases in micellar liquid chromatography, MLC, the retention of compounds is governed by hydrophobic and electrostatic forces. In the absence of electrostatic effects, the hydrophobicity of a compound is the predominant factor affecting its retention and its interaction with micelles. Because both interactions should be considered for ionic compounds, a novel retention model is proposed which includes the hydrophobicity of a compound and the molar fraction of its charged form. High correlations between the logarithm of the capacity factors and structural parameters were obtained for ionic compounds with different degrees of ionization. The effect of…

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Thermal Lens Spectrometric Detection of Catecholamines after Oxidation to Aminochromes

Abstract Experimental conditions for the spectrophotometric and thermal lens spectrometry (TLS) detection of catecholamines after oxidation to aminochromes with hexacyanoferrate (III) are optimized. At the low concentrations used in TLS, and in a 0.07 M citrate buffer, catecholamine oxidation can be performed at pH 7 and is immediate, whereas a lower pH value is required in spectrophotometry to avoid aminochrome polymerisation, the oxidation reactions being much slower. Similar TLS sensitivities are obtained for all catecholamines which facilitates HPLC evaluation. Sensitivity can be enhanced using a 50% ethanol-water medium. The linear dynamic range extends over two orders of magnitude, th…

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Determination of catecholamines as aminochromes by micellar liquid chromatography with thermal lens spectrophotometric detection

The determination of catecholamines (CAs) using micellar liquid chromatography with thermal lens spectrophotometric detection has been studied. CAs are oxidized with hexacyanoferrate(III) to aminochromes which are separated with a mobile phase of 0.05 M sodium dodecyl sulphate, 7% propanol and 0.03 M citrate buffer, pH 4.8, on a partially endcapped C18 column. The aminochrome-micelles and aminochrome-stationary phase association constants are evaluated. Using the 488 nm line of an Ar+ laser with 250 mW pump power the limits of detection are about 4 ng mL−1. The technique is applied to the determination of unconjugated CAs in urine using isoproterenol as internal standard.

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Determination of catecholamines in urine by micellar liquid chromatography with coulometric detection

The determination of catecholamines by HPLC with a sodium dodecyl-sulphate (SDS), micellar mobile phase on a C18 column and with coulometric detection was studied. The eluate was conditioned at +0.25 and +0.00 V, and the current at −0.16V was recorded. A previously developed model which describes the chromatographic behaviour of solutes in HPLC with hybrid, micellar mobile phases was used to optimize the SDS and ethanol concentrations. A mobile phase of 0.15M SDS in a phosphate buffer of pH 3.4 and without ethanol is recommended. The limits of detection were 0.4–0.7 ng ml−1. The procedure was applied to the determination of unconjugated L-dopa, norepinephrine and dopamine in urine. Direct i…

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