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Determination of tumor markers using carbon paste electrodes
Adámková, Hana ; Zima, Jiří (advisor) ; Fischer, Jan (referee)
In this master s thesis, electrochemical determination of homovanillic acid (HVA) andˈ vanillylmandelic acid (VMA) was performed on carbon paste electrode. The purpose of this thesis was finding out optimal conditions for determination of these analytes by ndifferential pulse voltammetry (DPV) and high pressure liquid chromatography with a carbon paste electrode as an electrochemical detector (HPLC-ED). The electrochemical behavior of the compounds depends mainly on pH of the solution; the best results are obtained in acidic medium. The limits of detection for DPV method were for HVA 0,38 μmol·dm-3 and for VMA 0,25 μmol·dm-3 . The limits of detection for HPLC-ED were for HVA 0,7 μmol·dm-3 and for VMA 0,2 μmol·dm-3 . Developed method was successfully used for the determination of homovanillic and vanillylmandelic acid in urine samples. With HPLC - ED the limits of detection 0,8 μmol·dm-3 (HVA) and 0,5 μmol·dm-3 (VMA) were achieved. Key words: Homovanillic acid, vanillylmandelic acid, carbon paste electrode, DPV, HPLC
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Optimalization and validation of method for electrochemical determination of triclosan
Vránová, Edita ; Dejmková, Hana (advisor) ; Fischer, Jan (referee)
In this thesis were, on the basis of earlier work, examined some of the conditions for the determination of triclosan by differential pulse voltammetry using carbon paste electrode and miniaturized carbon paste electrode. Phosphate buffer pH 11 was chosen as the most suitable medium of three supporting electrolytes with pH 11 and 12. The possibility of suppression of electrode passivation by addition of triton X-100 was studied. In addition, the validation parameters were searched, which included limits of detection, linearity of the concentration dependence, repeatability, and accuracy of the method. From these parameters, applicability of the method and the particular electrodes was assessed. Under the selected optimal conditions calibration curves for deionized, river and drinking water were measured. Detection limit with carbon paste electrode, was determined for deionized water to 120 ppb, for drinking water to 140 ppb and for river water to 90 ppb. The detection limit with miniaturized carbon paste electrode, was determined for the deionized water to 110 ppb , for drinking water to 130 ppb and for river water to 140 ppb. The linearity of the calibration curve was evaluated using the correlation coefficient. The samples of drinking and river water were then measured using carbon paste...
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The use of carbon-based electrodes for the development of new electrochemical methods for the determination of aminonitrophenols
Dejmková, Hana ; Zima, Jiří (advisor) ; Ludvík, Jiří (referee) ; Vytřas, Karel (referee)
4 ABSTRACT Methods for the determination of five isomers of aminonitrophenol were developed, based on the technique of differential pulse voltammetry (DPV) and HPLC with amperometric detection. As the working electrodes, boron-doped diamond film electrode (BDDFE) and glassy carvon paste electrode (GCPE) were employed. Preliminary electrode testing was performed by cyclic voltammetry. The methods were aimed to the determination of all five aminonitrophenol isomers in hair dyes and to the determination of 2-amino-4- nitrophenol and 4-amino-2-nitrophenol in body fluids after solid phase extraction. From the voltammetric methods, the one using BDDFE for the cathodic determination in hair dyes exhibits sufficient selectivity. The performance of chromatographic methods was found suitable for the determination of aminonitrophenols in both observed matrices. The applicability of the developed methods was successfully confirmed by the determination of tested analyted in real samples of hair dyes and spiked samples of urine. Preceding measurements are described, dealing with the determination of other oxidizable compounds, containing phenolic or aniline moieties on BDDFE. The obtained results confirm that in some cases, BDDFE shows more resistance to fouling than other carbon-based electrodes, but in most cases, the...
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Voltammetric determination of benzophenone-3 at carbon paste electrode
Molitor, Vít ; Zima, Jiří (advisor) ; Navrátil, Tomáš (referee)
A method for analysing benzophenone-3 on carbon paste electrode was developed. As a solvent a mixture Britton-Robinson buffer and methanol was used. The pH value of 12 was determined as optimal for further measurements. It was also found out that methanol added to the analyte solution did not negatively influence the voltammetric measurement. To decrease the limit of benzophenone-3 determination the accumulation of the analyte in the electrode surface was studied. The accumulation time of 300 seconds and accumulation potential of +400 mV were used as optimal. When measured under optimal coniditions the limit of detection was 6×10-7 M in deionised water and 5,5×10-7 M in drinking water. Real sample was measured using differential pulse voltammetry and spectrophotometry.
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The use of carbon-based electrodes for the development of new electrochemical methods for the determination of aminonitrophenols
Dejmková, Hana
4 ABSTRACT Methods for the determination of five isomers of aminonitrophenol were developed, based on the technique of differential pulse voltammetry (DPV) and HPLC with amperometric detection. As the working electrodes, boron-doped diamond film electrode (BDDFE) and glassy carvon paste electrode (GCPE) were employed. Preliminary electrode testing was performed by cyclic voltammetry. The methods were aimed to the determination of all five aminonitrophenol isomers in hair dyes and to the determination of 2-amino-4- nitrophenol and 4-amino-2-nitrophenol in body fluids after solid phase extraction. From the voltammetric methods, the one using BDDFE for the cathodic determination in hair dyes exhibits sufficient selectivity. The performance of chromatographic methods was found suitable for the determination of aminonitrophenols in both observed matrices. The applicability of the developed methods was successfully confirmed by the determination of tested analyted in real samples of hair dyes and spiked samples of urine. Preceding measurements are described, dealing with the determination of other oxidizable compounds, containing phenolic or aniline moieties on BDDFE. The obtained results confirm that in some cases, BDDFE shows more resistance to fouling than other carbon-based electrodes, but in most cases, the...
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Electrochemical determination of chlortoluron using carbon paste electrode
Houšková, Lucie ; Zima, Jiří (advisor) ; Vyskočil, Vlastimil (referee)
Chlortoluron is a herbicide from the group of substituted ureas and it is used for weed control in production of cereals and poppy. Substituted ureas are widely used but these substances are known for their high mobility in soil, persistence and contamination of underground water. Therefore, the development of analytical methods suitable for residual concentrations determination is necessary. This thesis deals with the determination of chlortoluron using carbon paste electrode (CPE) by the methods of differential pulse voltammetry and high-performance liquid chromatography with electrochemical (HPLC-ED) and spectrophotometric (HPLC-UV) detection. The aim of the work was to find optimal conditions suitable for chlortoluron determination. Further, the possibility of using miniaturized carbon paste electrode (mCPE) and usability of tested methods for determination of chlortoluron in model samples of river water and soil were studied. Concentration dependences in deionized water were measured by the method of DPV in the Britton-Robinson (BR) buffer (pH = 3) and methanol (10 %, v/v). The limit of detection was 3,7∙10-7 mol∙dm-3 in the case of CPE and 8,7∙10-8 mol∙dm-3 in the case of mCPE. Also, concentration dependences were measured using HPLC with mobile phase containing BR buffer (pH = 4) and...
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Determination of selected terpenoids by HPLC with electrochemical detection
Mužíková, Jana ; Dejmková, Hana (advisor) ; Schwarzová, Karolina (referee)
This thesis deals with the determination of carvacrol, thymol, and eugenol by HPLC with electrochemical detection. Carbon paste electrode and boron doped diamond film electrode were used as the working electrodes. For the comparison, UV spectrophotometric detection at 275 nm was used besides the electrochemical detection. The separation was performed on LiChroCART 125-4, RP-18e (5 µm) column. Optimum separation conditions were found: mobile phase consisting of acetonitrile and acetate buffer in ratio 50:50, the optimum buffer pH was pH 5. The optimum potential of working electrode during electrochemical detection was +0,8 V and +1,2 V for carbon paste electrode and boron doped diamond film electrode, respectively. For both electrodes, repeatability of the measurement was examined; the surface of both electrodes had to be renewed between the measurements. Under the obtained optimum conditions, calibration dependences were measured. The studied substances were determined in real samples, in Thymus vulgaris L. and Achillea millefolium L. and in thyme-containing tea and syrup.
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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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Determination of propyl gallate on carbon paste electrode
Vysoká, Marie ; Fischer, Jan (referee) ; Zima, Jiří (advisor)
Propyl gallate (PG) is a significant synthetic antioxidant and preservative. Its determination has been studied at carbon paste electrode (CPE) using differential pulse voltammetry (DPV) and high performance liquid chromatography with electrochemical detection (HPLC-ED) and with UV spectrometric detection (HPLC-UV). Concentration dependences were measured in the media of Britton-Robinson buffer (pH 5) and methanol (20 %, v/v) by DPV and the limit of detection 0,6110-7 moldm-3 was obtained. Using HPLC with a mobile phase consisting of 0,01 moldm-3 phosphate buffer (pH 4) and methanol (50 %, v/v) with potential of working electrode E = +0,8 V and detection wavelength λ = 280 nm, concentration dependences were measured. Limit of detection was determined to 0,39 moldm-3 for HPLC-ED and 4,95 moldm-3 for HPLC-UV. After verification of the extraction procedure PG was determined in vegetable oil. The resulting value of 3,2 mgkg-1 corresponds with permited limits.
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