|
| |
|
|
A new approach to the electroanalysis of primary bile acids and related steroids
Klouda, Jan ; Schwarzová, Karolina (advisor) ; Skopalová, Jana (referee) ; Vyskočil, Vlastimil (referee)
In this doctoral thesis, a novel method for the determination of primary bile acids cholic acid and chenodeoxycholic acid is presented. Bile acids play various vital roles in the mammalian body. Moreover, their determination is extremely helpful in liver and biliary disease diagnosis and management. These saturated organic compounds lack strong chromophores and fluorophores in their structure, and thus are usually hard to detect in spectroscopy. For this reason, either instrumentally advanced but expensive methods, such as mass spectrometry, or less reliable enzymatic methods are commonly employed in bile acids quantitation. Hence, the demand for simple and reliable methods for their determination is strong. Bile acids are also known to be virtually inert for direct electrochemical oxidation. Herein, a simple method for their chemical activation for electrochemical oxidation on bare electrode materials was developed, optimized and applied to cholic acid and chenodeoxycholic acid determination. The activation is based on a dehydration reaction of a primary bile acid with 0.1 mol L-1 HClO4 in acetonitrile (water content 0.55%) that introduces double bond(s) into the originally fully saturated steroid core. This naturally increases the electron density in the structure, and thus allows electrochemical...
|
|
|
Electrochemical oxidation of Bile Acids on Carbon Based Electrodes. The Possible Use in Electroanalysis.
Klouda, Jan ; Nesměrák, Karel (advisor) ; Zima, Jiří (referee)
The goal of this master's thesis was to examine the possibility of oxidation of seven selected bile acids and evaluate whether such processes are suitable for analytical purposes. The secondary goal was to describe the oxidation products of bile acid electrolysis. The experiments were carried out in a non-aqueous medium of acetonitrile and in a mixed medium of acetonitrile:water using linear sweep and cyclic voltammetry. The working electrode materials employed for voltammetric experiments were: highly oriented pyrolytic graphite, -cyclodextrin modified glassy carbon and boron doped diamond. Preparative electrolysis was carried out on a platinum electrode in the non-aqueous medium of acetonitrile. Experiments have shown that neither the highly oriented pyrolytic graphite electrode nor the -cyclodextrin modified glassy carbon electrode are suitable for analytical purposes under conditions used. The results achieved on the boron doped diamond electrode, on the other hand, have not yet been described in the literature. Primary bile acids cholic and chenodeoxycholic were oxidized at approximately 0.5 V lower potential in the mixed medium of acetonitrile:water than in the papers using carbon electrodes published until now. Products of oxidation on the platinum electrode were separated by TLC and...
|
|
|
Electrochemical Oxidation of Selected Bille Acids in Acetonitrile
Klouda, Jan ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
The use of voltammetry for determining bile acids and similar compounds is described in literature, but in most cases separation precedes. The goal of this bachelor's thesis was to develop a method for direct determination and identification of seven selected bile acids. The experiments were carried out in non-aqueous medium of acetonitrile using DC voltammetry. As the working electrode a rotating disc platinum electrode and a rotating disc glassy carbon electrode were employed. Platinum electrode proved not to be suitable for this kind of use. The GCE on the other hand showed some potential, but the chemical properties of the bile acids exclude its use in terms of identification.
|
|
| |
guest ::
RSS feed.