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Analysis of nutritionally important substances in fruit tree waste products by HPLC
Šírová, Karolína ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Karolína Šírová Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: Mgr. Anežka Adamcová Title of Diploma Thesis: Analysis of nutritionally important substances in fruit tree waste products by HPLC This diploma thesis deals with the content of phenolic compounds in various parts of tree of the genus Pyrus. The theoretical part is focused on characterization, biosynthesis, chemical and biological properties of major phenolic compounds in pear-trees and the possibilities of their determination with the use of the latest scientific studies. The experimental part contains an extensive analysis of arbutin, chlorogenic acid, 1,5- dicaffeoylquinic acid, 3,5- dicaffeoylquinic acid and rutin in extracts of leaves, bark, buds, fruits, flowers and wood chip. Developed and validated HPLC-DAD method was used and the total antioxidant activity was determined by FIA method with electrochemical detection. An ASCENTIS Express RP-Amide 150×4.6 mm, 2.7 μm analytical column and gradient elution consisting of organic part of acetonitrile (ACN) and water part with 0,85% phosphoric acid (pH = 2.2) were used for analysis. The detection was performed by DAD detector at wavelengths 220 nm, 327 nm and 354 nm. The...
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Monitoring the profile of phenolic substances in different parts of apple trees by HPLC
Šilhavá, Kristýna ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Kristýna Šilhavá Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: Mgr. Anežka Adamcová Title of Diploma Thesis: Monitoring the profile of phenolic substances in different parts of apple trees by HPLC This diploma thesis covers the performance of a quantitative analysis of phenolic compounds in ten different cultivars in Malus. Specifically, the presence of phloridzin, phloretin, rutin, quercitrin and chlorogenic acid was monitored. Extracts of buds, flowers, leaves and bark in each species were analyzed during the four different vegetation periods. Further, the presence of phenolic compounds in samples of wood chips and fruits was monitored. The determined analytes displayed a different content profile depending on the plant material, apple cultivar and the period in which they were collected. Except for fruits, phloridzin was the dominant component in all varieties and in all materials. The highest total concentration of phenolic compounds was found in the leaves in the spring March-April 2020 in species 'Rubinstep'. This diploma thesis used a developed and validated HPLC-DAD method for a large number of extracts. A YMC-Triart C18 ExRS column (150 × 4.6 mm × 5 µm, 8 nm) was chosen...
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HPLC determination of lutein, vitamin E, vitamin E acetate, beta-carotene in food supplements
Hrdinová, Petra ; Šatínský, Dalibor (advisor) ; Chocholouš, Petr (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Petra Hrdinová Consultant. Doc. RNDr. Dalibor Šatínský, Ph.D. Rigorous thesis title: HPLC determination of lutein, vitamin E, vitamin E acetate, beta-carotene in food supplements The rigorous thesis deals with optimization of conditions for determination of lutein, beta-carotene and vitamin E , and vitamin E acetate in food supplements Ostrovidky, Ocutein forte, Walmark Lutein forte, Ocumax, Avilut, Ocuvite lutein forte, Lutein for eyes, Walmark betacarotene and Revital Super Betacarotene. High performance liquid chromatography (HPLC) was used for determination. Three chromatographic columns were tested, the best results were obtained using an Ascentis Express C-18 column 100 x 4.6 mm with a particle size 5 microns. Detection was performed by UV/Vis at a wavelength of 290 nm for vitamin E and E acetate, and 450 for lutein and beta-carotene. Separation was carried out by gradient elution with mobile phase of acetonitrile + methylenchlorid:hexane (1:1). Flow rate of the analysis was 1 ml/min and column temperature was set at 30 řC. Volume of sample injection was 5 µl. The analysis time lasted 9 minutes. The results of the determination of the content of lutein, beta-carotene and vitamin E in...
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Development of HPLC method for analysis of food supplements based on berberine extract
Zíka, Jan ; Šatínský, Dalibor (advisor) ; Khalikova, Maria (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Jan Zíka Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Development of HPLC method for analysis of food supplements based on berberine extract In this diploma thesis, an HPLC method for the determination of berberine and its related isoquinoline alkaloids aromoline, berbamine, magnoflorine, tetrahydropalmatine, jatrorrhizine, palmatine, tetrahydroberberine and oxyberberine was developed and validated. The method was subsequently applied to the determination of the relevant analytes in the food supplements Allnature Berberin 98% extract, Ostrovit Berberin, Swanson Berberin and GreenFood Berberine. An Ascentis® Express AQ-C18 (150 x 4.6 mm, particle size 2.7 µm) analytical column was used for chromatography analysis, using an acetonitrile/0.085% aqueous solution of phosphoric acid mobile phase. The flow rate of mobile phase was 1 ml/min with a sample injection volume of 5 µl and a column temperature of 30 řC. The gradient elution was used for analysis and detection was performed with a DAD detector at wavelengths of 225 and 345 nm. Key words: HPLC, berberine, aromoline, magnoflorine, berbamine, palmatine, tetrahydropalmatine, jatrorrhizine, tetrahydroberberine,...
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Studying the distribution of substituents in derivatives based on hyaluronane
Sedláček, Jakub ; Šatínský, Dalibor (advisor) ; Zimčík, Petr (referee) ; Chmelař, Josef (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Ing. Jakub Sedláček Supervisor doc. RNDr. Dalibor Šatínský, Ph.D. Title of Doctoral Thesis Studying the distribution of substituents in derivatives based on hyaluronan Derivatives based on hyaluronan have found applications in various areas of medicine. Prepared derivatives are commonly characterized by their molar mass and their degree of substitution, however, such parameters are unable to distinguish among derivatives with different distributions of substituents along the chain, which may exhibit different macroscopic properties. For this reason, methods to determine the distribution of substituents along the chain are needed. The presented thesis deals with the determination of distribution of amino groups in deacetylated hyaluronan. The theoretical part starts with a description of hyaluronan structure and of its derivatives. Next, the application, the preparation, and the characterization of deacetylated hyaluronan are discussed, focusing particularly on its depolymerisation into oligosaccharides using deaminative cleavage or enzymes that degrade hyaluronan. Finally, examples of liquid chromatographic methods used to analyse hyaluronan oligosaccharide are presented. The experimental part...
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Monitoring the profile of phenolic substances in different parts of apple trees by HPLC
Šilhavá, Kristýna ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Kristýna Šilhavá Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: Mgr. Anežka Adamcová Title of Diploma Thesis: Monitoring the profile of phenolic substances in different parts of apple trees by HPLC This diploma thesis covers the performance of a quantitative analysis of phenolic compounds in ten different cultivars in Malus. Specifically, the presence of phloridzin, phloretin, rutin, quercitrin and chlorogenic acid was monitored. Extracts of buds, flowers, leaves and bark in each species were analyzed during the four different vegetation periods. Further, the presence of phenolic compounds in samples of wood chips and fruits was monitored. The determined analytes displayed a different content profile depending on the plant material, apple cultivar and the period in which they were collected. Except for fruits, phloridzin was the dominant component in all varieties and in all materials. The highest total concentration of phenolic compounds was found in the leaves in the spring March-April 2020 in species 'Rubinstep'. This diploma thesis used a developed and validated HPLC-DAD method for a large number of extracts. A YMC-Triart C18 ExRS column (150 × 4.6 mm × 5 µm, 8 nm) was chosen...
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Optimization of the screening strategy for the detection of so-called new drugs of the synthetic cannabinoid group
Ozsvaldová, Silvia ; Šatínský, Dalibor (advisor) ; Plachká, Kateřina (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Silvia Ozsvaldová Supervisor: prof. RNDr. Dalibor Šatínský Ph.D. Consultant: PharmDr. Viktor Voříšek Titel of diploma thesis: Optimization of the screening strategy for the detection of so-called new drugs of the synthetic cannabinoid group Our diploma thesis pursues the main aim of optimizing the screening strategy of the capture of synthetic cannabinoids. In the theoretical part, we described the history of synthetic cannabinoids, their classification, and their effects on human health status. Next, we describe the determination, using the ultra-high liquid chromatography joined with mass spectrometry, which uses the principle of OrbitrapTM as a mass analyzer. We performed on our spiked sample of the JWH-018 N-(4-hydroxypentyl) on three different columns in the experimental part. There were Phenyl Hexyl Kinetex®, Luna Omega® Polar C18 and Arion® Polar C18 UHPLC columns. Also, we performed specific PRM scans on Luna and Arion columns. Samples on all three columns were measured in triplets, in duplicate during the PRM. We constructed calibration dependences, based on acquired values from which the parameters LOD and LOQ were calculated. Subsequently, we present these analytical control quality...
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Optimization of conditions for qualitative and quantitative analysis of farnesol and tyrosol using UPLC-MS/MS.
Greguš, Petr ; Nováková, Lucie (advisor) ; Šatínský, Dalibor (referee)
Direct activation of C-H bond in tetrazoles Richard Lubojacký, 5th grade Supervisor: Prof. RNDr. Milan Pour, Ph.D. Department of Inorganic and Organic Chemistry, Faculty of Pharmacy in Hradec Králové Within the framework of this diploma thesis, direct arylation and alkenylation of 1- substituted tetrazoles at C5 was developed and optimized. An economical preparation of a range of 1,5-disubstituted tetrazoles was thus made possible. In these reactions, Pd-catalysis in the presence of CuI and Cs2CO3 was found as optimal. Contrary to similar reactions of imidazoles and purines, it was necessary to incorporate phosphine ligands in order to stabilize Pd - intermediates and prevent them from a premature decomposition into cyanamides. A library of 1,5-disubstituted tetrazoles with very promising yields has been prepared using this method.
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