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Voltammetry at Silica Gel-Modified Carbon Paste Electrode
Šestáková, Ivana ; Navrátil, Tomáš
Voltammetry using silica gel modified carbon paste electrode (SiO2-CPE) for oxidation of selected flavonoid showed better sensitivity and reproducibility than oxidation using glassy carbon or unmodified carbon paste electrode. Only SiO2-CPE is useful for study of cadmium complexation with cysteine containing ligand as phytochelatin or metallothionein. Voltammetry on boron doped diamond electrode showed only peak of sulfur compound oxidation, which decreased with the addition of cadmium ions.
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Behavior of Metallothioneins and Phytochelatins at Mercury and Amalgam Electrodes
Šestáková, Ivana ; Navrátil, Tomáš ; Josypčuk, Bohdan
The presence of cysteine residues in molecules of metallothioneins or phytochelatins is crucial for their electrochemical behavior. At mercury electrodes, the reduction of\ntetracoordinated Cd and Zn in molecule of mamamalian MT is observed in solution of pH 8- 8.5, whereas with lowering pH or at presence of excessive ions, signals of differently coordinated or free metal ions appear. Such changes were confirmed on model complexes with phytochelatin PC2 .Using amalgam electrodes CuSAE or AgSAE for voltammetry of metallothioneins or phytochelatins, their Cu or Ag complexes are formed on the electrode surface, which could be with limitations - employed for the analytical purposes.
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Determination of Sibiromycin by UPHLC Method
Šestáková, Ivana ; Čabala, Radomír (referee)
A new separation and quantification method using ultra high-performance liquid chromatography (UHPLC) with UV detection was developed for the detection of sibiromycin in fermentation broth of Streptosporangium sibiricum. The solid phase extraction method based on cation-exchange was employed to pre-concentrate and purify fermentation broth containing sibiromycin prior to UHPLC analysis. The whole assay was validated and showed a linear range of detector response for the quantification of sibiromycin in a concentration from 3.9 to 250.0 µg/ml, with correlation coefficient of 0.999 and recoveries rating from 71.66±3.55 % to 74.75±5.18 %. Method limit of quantification of the assay was determined as 0.18 µg/ml and was verified with resulting RSD of 9.6 % and accuracy of 97.6 %. The developed assay was used to determine the sibiromycin production in 12 different fermentation broths. Moreover, several natural sibiromycin analogues/derivatives were described with pilot characterization using off-line mass spektrometry.
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Determination of aminoglutethimide using HPLC-ED on carbon pastes
Vlachová, Karolína ; Šestáková, Ivana (referee) ; Zima, Jiří (advisor)
In this thesis, the determination of AGT, sooner used as anticancer drug, especially for the treatment of breast cancer in postmenopausal women or for the treatment of prostate cancer, by high performance liquid chromatogramy with UV spectrophotometric detection (HPLC-UV) and electrochemical detection (HPLC-ED) on carbon paste electrodes (CPEs) was studied. CPEs were prepared from glassy carbon microspheres and different pasting liquids - routinely used mineral oil (CPE-MO) and less commonly used tricresylphosphate (CPE-TCP) and silicone oil (CPE-SO). The concentration dependences of AGT were measured by HPLC-UV with detection wavelength 242 nm, by HPLC-ED with a working potencial of +1,3 V for CPE-MO and + 1,1 V for CPE-TCP in mobile phase containing phosphate buffer (pH 4) and methanol 50:50 (v/v). The following limits of detection were achieved - 3,6. 10-7 mol.l-1 for UV spectrophotometric detection, 2,5. 10-7 mol.l-1 for electrochemical detection with CPE-MO and 9,7. 10-7 mol.l-1 for electrochemical detection with CPE-TCP. AGT was also determined in model samples of urine. With HPLC-UV it was not possible to detect AGT, because of the interferences of other compounds. With HPLC-ED on CPE-MO the limit of detection 5,2. 10-7 mol.l-1 AGT was achieved. KEY WORDS Aminoglutethimide HPLC with UV...
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