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Sequential injection chromatography - advanced separations of bioflavonoids in food supplements
Pavelková, Kristýna ; Chocholouš, Petr (advisor) ; Šatínský, Dalibor (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical chemistry Candidate: Kristýna Pavelková Supervisor: doc. PharmDr. Petr Chocholouš, PhD. Title of diploma thesis: Sequential injection chromatography - advanced separations of bioflavonoids in food supplements Two methods were developed in the thesis. A primary method of sequential injection chromatography with UV detection was developed for separation of bioflavonoids rutin, hesperidin and diosmin. A second method was developed for adjustment data, which enables to increase sensitivity of first developed method. Chromatographic column YMC-Triart C18 ExRS; 100 mm 4.6 mm; 5 μ, 8 nm was used for separation. The mobile phase consisted of a mixture of acetonitrile with phosphoric acid solution pH 2.0 prepared in a ratio of 25:75. Isocratic elution was chosen; flowrate was 10 μl/s and total length of analysis was 7.9 minutes. Sequential injection chromatography system and computer software SIAsoft was used for analysis. Programs Microsoft Excel and Origin Pro 9 were used for processing and adjustment of data. Developed method was not succesfull in quantification of amount of flavonoids in Hemostop Probio MAX. Method for data adjustment enabled significant reduction of LOD and LOQ. Keywords: flavonoids, rutin,...
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Modern extraction techniques in connection with HPLC for analysis of contaminants
Kholová, Aneta ; Šatínský, Dalibor (advisor) ; Ventura, Karel (referee) ; Malíř, František (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Training Workplace Department of Analytical Chemistry Doctoral Degree Program Bioanalytical Methods Candidate Mgr. Kholová Aneta Supervisor prof. RNDr. Dalibor Šatínský, Ph.D. Advisor PharmDr. Ivona Lhotská, Ph.D. Title of Doctoral Thesis Modern extraction techniques in connection with HPLC for analysis of contaminants A compilation of six publications is presented in this dissertation thesis. The work focuses on applying and comparing extraction sorbents to analyze contaminating substances in food and food supplements. The main aim of this thesis was to present micro and nanofibers as suitable extraction sorbents for use in analytical chemistry. For this purpose, the fibers were compared with other, mostly commercial, extraction sorbents suitable for the type of matrix tested. All experiments were carried out in the on-line connection of the extraction sorbent through the selection valve with the analytical column in the chromatographic system. A crucial part was also the use of the extraction properties of nanofibers for the analysis of real-life samples. In the first part, the extraction efficiency was studied on liquid matrices, where no need for complex matrix purification was required. The main aim was sufficient retention and...
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Advanced extraction materials for sample preparation in chromatographic analysis
Zatrochová, Slavomíra ; Šatínský, Dalibor (advisor) ; Solich, Petr (referee) ; Ševčík, Juraj (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Training Workplace Department of Analytical Chemistry Doctoral Degree Program Pharmaceutical Analysis Candidate Mgr. Slavomíra Zatrochová Supervisor Prof. RNDr. Dalibor Šatínský, Ph.D. Advisor PharmDr. Ivona Lhotská, Ph.D. Title of Doctoral Thesis Advanced extraction materials for sample preparation in chromatographic analysis The submitted dissertation presents an annotated set of publications focusing on advanced extraction materials in analytical chemistry and their prospective use as sorbents in sample preparation prior to HPLC analysis. The work was created based on the cooperation with the Technical University of Liberec and the University of Valencia in Spain. In the first part, a new sorbent based on a hybrid monolith with a metal-organic framework (MOF) was developed for conventional Teflon-coated magnetic stir bars, and the resulting hybrid monolith was evaluated as a stir bar sorptive extraction (SBSE) sorbent for the extraction of estrogens in water and urine samples. In the second part, the work was focused on nanofibrous and microfibrous polymers and the production of fibers by alternating current (AC) electrospinning. The extraction efficiency, selectivity and stability of different polymer nanofibers were tested. The...
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Study of BTEX determination by microextraction in the Lab-in-syringe system coupled with gas chromatography
Kohániová, Andrea ; Horstkotte, Burkhard (advisor) ; Šatínský, Dalibor (referee)
Charles university Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Andrea Kohániová Supervisor: M.Sc. Burkhard Horstkotte, Ph.D. Co-supervisor: PharmDr. Ivana Horstkotte Šrámková, Ph.D. Title: Study of BTEX determination by microextraction in the Lab-in-syringe system coupled with gas chromatography Benzene, toluene, ethylbenzene and xylenes are one of the major contaminants in the environmental water samples. Because these compounds are consider to be toxic to humans by World Health Organisation, their determination is critically important. The determination of BTEX using gas chromatography with flame ionisation detection combined with direct single drop microextraction using Lab-in-syringe system was studied. The effective paramateres such as microdroplet volume, extraction time, type and use of salt solution and chromatographic parameters were evaluated. The purpose of this work was automation of the entire process using 3D elements in the system.
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Quality control of food supplements with melatonine using separation methods
Chalupníková, Natálie ; Šatínský, Dalibor (advisor) ; Lhotská, Ivona (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Natálie Chalupníková Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Quality control of food supplements with melatonine using separation methods In this diploma thesis, an HPLC method was developed and validated for the simultaneous determination of melatonin and pyridoxine. The developed method was applied to the determination in food supplements, Tozax Sleep Trip (mcePharma s. r. o.), Clinical Melatonin B6 syrup (Clinical nutricosmetics s. r. o.), Fast Sleep oral spray with melatonin (EmergoPharm Sp. z o. o. Sp. K.), Melatonin Rapid complex 5 mg ODT (Salutem Pharma s. r. o.), Allegra Melatonin 3 mg (Woykoff a. s.), Clinical Melatonin Forte (Clinical nutricosmetics s. r. o.), Melatonin 2 mg (Allnature s. r. o.), Melatonin new extra 5 mg (Nutricius s. r. o.), Clinical Melatonin B6 Gummies (Clinical nutricosmetics s. r. o.). The method was based on the use of a SUPELCO Ascentis Express C-18 chromatography column (100*4.6 mm, particle size 2.7 µm). The separation was carried out under gradient elution, using a mobile phase of acetonitrile and 0.085% phosphoric acid at pH 2.2, flow rate 1 ml/min and constant temperature 30řC. A detection wavelength of 278 nm was chosen...
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Solid phase extraction using nanofibrous sorbents prior to liquid chromatography for determination of drugs and contaminants
Nastoupilová, Jana ; Lhotská, Ivona (advisor) ; Šatínský, Dalibor (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Jana Nastoupilová Supervisor: PharmDr. Ivona Lhotská, Ph.D. Title of diploma thesis: Solid phase extraction using nanofibrous sorbents prior to liquid chromatography for determination of drugs and contaminants The diploma thesis is focused on the optimization of a new type of solid-phase extraction (SPE) using nanofibrous sorbents filled in centrifugal filters for the determination of contaminants (bisphenols) and drugs. The aim is to increase the quantity of parallel analyses. The composite polymer nPCL/µPCL (nano and microfibers of polycaprolactone) was chosen as the tested sorbent because of its promising results in previous works. The aim of the diploma thesis was optimization of conditions for extraction and validation of the method. The method of choice was microextraction, when discs from nanofibrous sorbent were cut and then filled in centrifugal filters. A centrifuge was used for passing liquid through the sorbent. Analysis was carried out by UHPLC (chromatography column YMC-Triart C18 ExRS, size 100x4.6 mm, particle size 3 µm) and detection was performed by DAD detector (210 and 220 nm). During the optimization, number of nanofibrous discs filled in centrifugal filters, volume of...
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Control of mycotoxin content in food supplements
Přívratská, Nikola ; Šatínský, Dalibor (advisor) ; Kujovská Krčmová, Lenka (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Nikola Přívratská Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Control of mycotoxin content in food supplements Due to the growing popularity of nutraceuticals, some concerns about their quality and safety have been expressed. The presented work describes the development of a fast method for mycotoxin ochratoxin A (OTA) determination using high performance liquid chromatography (HPLC) and column switching technique in combination with on-line solid phase extraction (SPE). The method was used for direct determination of OTA in milk thistle-based nutraceuticals. Nutraceuticals were extracted by methanol - water solution in a ratio of 1:9. A volume of 50 μl of the extracted sample was injected on the extraction column Ascentis Express RP-Amide (5 x 2.1 mm, 5 µm particle size). The sample was cleaned from interfering compounds with 20% methanol at a flow rate of 1 ml/min. After a period of 1 minute the valve was switched and mobile phase eluted OTA trapped on the extraction column to the analytical column. Separation was performed by gradient elution on the Ascentis Express Phenyl-Hexyl (100 x 4.6 mm, 5 µm particle size) column using a mobile phase consisting of...
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HPLC in quality control of food supplements based on curcumine extracts
Stříbrná, Veronika ; Šatínský, Dalibor (advisor) ; Solich, Petr (referee)
Charles University, Faculty of Pharmacy in Hradec Kralove Department of Analytical Chemistry Candidate: Veronika Stříbrná Supervisor: prof. RNDr. Dalibor Satinsky, Ph.D. Title of diploma thesis: HPLC in quality control of food supplements based on curcumin extracts In this diploma thesis, a new HPLC method for the simultaneous determination of active components in food supplements, piperine, curcumin, demethoxycurcumin and bisdemethoxycurcumin was developed and validated. The method was used to determine the level of the relevant analytes in the selected food supplements, namely Curcumin - piperine plus Vieste, Curcumin-piperine complex Natural Medicaments, Turmeric: piperine Setaria, Cur-Cum Astina, Curcumin Liftea, Curcumin Advance a Curcumin turmeric. Finally, the obtained results were compared with the declared extract content and evaluated as a percentage of quality of the food supplement. An Ascentis® Express RP-Amide 150 x 4,6 mm, 2,7 µm particle size analytical column with Ascentis® RP-Amide 5 x 4,6 mm, 2,7 µm particle size precolumn was used for analysis. A gradient elution with analysis time of 12.5 minutes and flow rate of mobile phase 1.0 ml/min was used. As the mobile phase a mixture of acetonitrile 100% and 0.1% phosphoric acid was chosen. The detection was performed with a DAD...
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Development of UHPLC-DAD method for separation of phenolic substances in plant material and extraction optimization
Turčanová, Anna ; Sklenářová, Hana (advisor) ; Šatínský, Dalibor (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Anna Turčanová Supervisor: doc. PharmDr. Hana Sklenářová, Ph.D. Advisor: Mgr. Marcela Hollá Title of the diploma thesis: Development of UHPLC-DAD method for separation of phenolic substances in plant material and extraction optimization This diploma thesis deals with development of UHPLC-DAD method for separation of selected phenolic substances (arbutin, chlorogenic, neochlorogenic, cryptochlorogenic, isochlorogenic A and caffeic acid, cynarin, catechin, epicatechin, rutin, hyperoside, hirsutrin, reynoutrin, guaiaverin, quercitrin and quercetin). UHPLC analysis of these phenolic substances took place on a Luna® Omega Polar C18 100 (150 x 2.1 mm; 1.6 μm) column with fully porous particles. As a part of the optimization method, a column with core-shell particles (Kinetex® Polar C18) and a column with a hybrid stationary phase (YMC-Triart C18 ExRS) were also tested. The sample injection volume was 2 μl, the flow rate has been set to 0.3 ml/min and temperature of the column has been set to 30 řC. As a mobile phase ultrapure water acidified with acetic acid to pH 2.8 in combination with acetonitrile has been used. The total analysis time was 17.5 min and detection was performed using a DAD detector at...
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