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The influence of Quantum Dots Particles to cChemiluminiscence Based on Oxidation by Permanganate
Kořínková, Martina ; Sklenářová, Hana (advisor) ; Šatínský, Dalibor (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Kořínková Supervisor: Doc. PharmDr. Hana Sklenářová, Ph.D. Title of Rigorosis Thesis: The influence of Quantum Dots particles to chemiluminiscence based on oxidation by permanganate Quantum Dots (QDs) particles are semiconductor nanocrystals, which have become attractive for many scientific institutions for its unique optical and physical properties. In this thesis it was found out, whether QDs have any effect on the intensity of chemiluminescence at the reaction with potassium permanganate in sulfuric acid medium. QDs with emission maxima at 520, 575, 603 a 636 nm were tested, QDs solutions were added subsequently to the chemiluminescent system, where the oxidized analytes were organic compounds such as gallic acid, hydroquinone, pyrocatechol, resorcinol and phloroglucinol. Achieved results were then compared with the measurement without addition of QDs to the chemiluminescent system. The experiment was performed by the flow method sequential injection analysis (SIA). Obtained results showed, that the highest growth of intensity of chemiluminescence was recorded using QDs with emission maximum at 520 nm, the procentual growth of the intensity of CL ranged to 26,73 %. The...
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Study of Sample Matrix Effect for SIA Determination of Aluminium in Real Samples
Fialová, Barbora ; Sklenářová, Hana (advisor) ; Matysová, Ludmila (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department: Department ofAnalytical chemistry Candidate: Mgr. Barbora Fialová Consultant: Assoc. Prof. PharmDr. Hana Sklenářová, Ph.D Title of Thesis: Study of sample matrix effect for SIA determination of aluminium in real samples This rigorosis thesis represents a continuation of diploma thesis in which spectrophotometric detection of aluminium after complex formation with aluminon based on method described in ČSN 83 0520 part 22 B was studied. During the reaction colour product was formed. The reaction was transferred into SIA system and the reaction conditions were optimised. After that, several real water samples were measured. During the recovery evaluation some effects of sample matrix influencing the determination were found. Identification and elimination of these influences are the aims of this rigorosis thesis. ČSN 83 0520 was used to select the ions, which could influence aluminium complexation with aluminon. In case of common ions testing after completed interference study the influence of these ions for the measurement was studied. We discovered, that the detection is influenced by fluorides, ferrous and ferric ions. Fluorides are present in potable water in a very low concentrations and influence of ferrous and...
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Optimization of chromatographic separation for the determination of 4-aminophenol and active substances in Valetol
Daňková, Jana ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
This thesis deals with the optimization of separation conditions determine paracetamol, caffeine, propifenazone and 4-aminophenol in Proprietary Medicinal Products Valetol. As an analytical method was chosen HPLC with UV detection mainly for the following reasons: many other tablets contain excipients which are from the sample during analysis impossible, and separated themselves determination of active substances to monitor the stability of active substances The work was conceived as original, and the emphasis is on the greatest possible simplicity and less time consuming and optimized separation while maintaining high accuracy and reliability of the method. Optimal conditions suitable for the final validation of the separation were found on a column of C-18 RP-amide. Total analysis time does not exceed 13 minutes with equilibration after gradient elution of the column to its original condition. All substances are separated with a resolution greater than 1.5. The peaks of substances are symmetric and do not show significant peak tailing besides AMF. The zero line is despite the gradient elution stable.
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Determination of selected phenolic compounds in fruit
Pechová, Martina ; Sklenářová, Hana (advisor) ; Šatínský, Dalibor (referee)
Charles University Faculty of Pharmacy in Hradci Králové Department of Analytical Chemistry Candidate: Bc. Martina Pechová Supervisor: Doc. PharmDr. Hana Sklenářová, Ph.D. Title of Diploma Thesis: Determination of selected phenolic compounds in fruit This diploma work deals with development and optimization of HPLC method for determination of selected phenolic compounds - gallic acid, chlorogenic acid, caffeic acid, catechin, epicatechin, rutin, quercetin, quercitrin, phloretin and phloridzin. The diploma work includes information about the general characteristics of phenolic compounds and information about their structure. It further describes HPLC method and mentions the short review of scientific publications regarding this topic. In the optimization step several types of gradients of mobile phase, stationary phase (chromatographic column of type C18, phenyl-hexyl, biphenyl, amino, cyano and monolithic column), other separation conditions (temperature, extraction) were tested and validation of the method was carried out. For the analysis of selected compounds precolumn Ascentis Express C18 (5 x 4,6 mm x 5 µm) and the column Kinetex C18 column (150 x 4,6 mm x 5 µm) were used. The detection was performed by DAD spectrophotometric detector at wavelengths of 255, 280, 320 and 365 nm, column...
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Development of extraction procedure for determination of tocopherols
Klabačková, Sáva ; Kujovská Krčmová, Lenka (advisor) ; Sklenářová, Hana (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Sáva Klabačková Supervisor: RNDr. Lenka Kujovská Krčmová, Ph.D. Title of diploma thesis: Development of extraction procedure for determination of tocopherols In the present work liquid-liquid extraction for determination of alpha, beta, gamma and delta tocopherol from human serum was developed miniaturized. Individual extraction steps as deproteinization, centrifugation, evaporation and final filtration were optimized. Solid supported liquid extraction (SLE) was also tested for determination of tocopherols and seems to be very promising for use in bioanalysis. During the miniaturization of the extraction procedure the main emphasis was placed on simplicity, speed and low consumption of samples and solvents. Method was also partly validated. The new extraction process is part of an already developed UHPLC method for the determination of individual forms of tocopherols and will serve to determine the antioxidant capacity of cancer patients during the chemotherapy treatment. Key words: tocopherols, LLE, SLE, biological material
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HPLC application in pharmaceutical analysis
Bajcurová, Lucie ; Matysová, Ludmila (advisor) ; Sklenářová, Hana (referee)
The HPLC method for determination of ketoprofen in therapeutic preparations "PRONTOFLEX" - a 10% skin spray and "Ketonal" - a 5% cream has been developed. This method was based on already developed and validated method for analyzing the preparation "KETOPROFEN" - a 2.5% gel. Both of the methods have been developed in the same department. The chromatographic separation was performed on SUPELCO Discovery C18 column (125 mm x 4.6 mm, 5 µm). The mobile phase consisted of a mixture of acetonitrile, water and a phosphate buffer pH 3.5 (40:58:2, v/v/v). At a mobile phase flow rate of 1.0 ml/min, injection volume of 10 μl and UV detection at a wavelength of 233 nm, the total time of analysis was less than 10 minutes. Ethylparaben was used as an internal standard.
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Vývoj optického sensoru pro salicylát
Soukupová, Marie ; Matysová, Ludmila (advisor) ; Sklenářová, Hana (referee)
We dealt with the development of optical sensor for salicylate. Sensing layer of sensor was based on metalloporphyrins. Metalloporphyrins embody great optical features. Metalloporphyrins are commonly employed as ionophores in ion-selective electrodes (ISEs). Observations from work with ISEs are applied to optical sensors. At first, membrane was constructed, based on tetraphenylporphyrin copper(II) (Cu(TPP)) and it did not show significant sensitivity towards salicylate. Further there were membranes created from tetraphenylporphyrin manganese(III)chloride (Mn(TPP)) and gallium(III)phthalocyanine chloride (Ga(PC)). Reactivity of Mn(TPP) was comparable with reactivity of Cu(TPP). Membrane from Ga(PC) displayed considerable reactivity and sensitivity towards salicylate. Later the membrane's capability was tested to detect valproate. We discovered that the limit of detection for valproate is much lower than for salicylate. Due to great reactivity and variability in membrane response in spectrophotometric assay we were not able to set the working conditions for application to flow system and to dissolution as well. Ga(PC) has thus very good potential in use for detection of valproate. Valproate is one of the most used antiepileptic drugs.
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Study of quinone and Quantum Dots particles effects on chemiluminescence reaction
Kořínková, Martina ; Sklenářová, Hana (advisor) ; Šatínský, Dalibor (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Martina Kořínková Supervisor: PharmDr. Hana Sklenářová, Ph.D. Title of Diploma Thesis: Study of quinone and Quantum Dots particles effects on chemiluminescence reaction A purpose of this Diploma Thesis was to observe and interpret the influence of 9,10- phenanthrenequinone, dithiothreitol and Quantum Dots (QDs) on chemiluminescent (CL) system, which contained hydrogen peroxide, luminol and potassium ferricyanide. All analyses were performed by the flow method of sequential injection analysis (SIA). The chemiluminescent emission of luminol was based on its oxidation by hydrogen peroxide during the catalysis by FeIII (CN)6. There is also different CL system, which has been developed by Japanese scientists, consisting quinone, luminol and dithiothreitol. The interest of this thesis was reproducing the results, which were reached by authors of the Japanese study, however with the use of SIA method the results of measurements were not comparable. The 9,10-phenanthrenequinone influenced the CL signal in the sense of shortening the emission length and thereby it is possible to evaluate the difference between the sizes of peak area in single measurements. The solution of dithiothreitol...
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