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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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HPLC in quality control of food supplements containing gingerols and curcumins
Hujová, Eliška ; Šatínský, Dalibor (advisor) ; Chocholouš, Petr (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Eliška Hujová Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: HPLC in quality control of food supplements containing gingerols and curcumins In this diploma thesis, a new HPLC method for determination of 6-, 8- and 10-gingerol, 6-shogaol, curcumin, demethoxycurcumin, bisdemethoxycurcumin, and piperine was developed and validated. The developed method was used for the analysis of food supplements: Kurkumin - piperin plus (+ zázvor) from VIESTE, Bio tumeric + ginger from VANAVITA, Ginger root extract from BioMedical, Shogaol zázvor from EPIGEMIC®, Ginger root extract from SWANSON®, and Ginger root (Zingiber officinale) from SOLGAR®. Just as a matter of interest, this method was applied for the selected tea blends containing ginger and/ or tumeric: Dilmah Orange & Ginger (flavoured ceylon black tea), Loyd Brusinky & Zázvor, Teekanne Dýchací cesty a krk se zázvorem, Pickwick Nos a krk se zázvorem, Tesco Ginger & Lemon, Teekanne Ginger Curcuma. For the analysis YMC-Triart C18 ExRS (150 x 4.6 mm; 3 µm) analytical column was used. Separation was carried out by gradient elution with mobile phases A: acetonitrile, B: ultrapure water at flow rate 1 ml/min. Detection was...
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The use of HPLC technique in the analysis of phenolic compounds in plant material of fruit trees
Adamcová, Anežka ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee) ; Vávra, Radek (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Anežka Adamcová Supervisor: Prof. RNDr. Dalibor Šatínský, Ph.D. Title of the Dissertation Thesis: The use of HPLC technique in the analysis of phenolic compounds in plant material of fruit trees Although fruits are well studied and known for their high content of antioxidants and positive health benefits, the main aim of the presented dissertation thesis consists in the characterization of biological active compounds in individual parts of fruit tree material (leaves, bark, buds, flowers, and wood chips). The theoretical part is focused on fruit trees and the characterization of phenolic compounds. Their properties and the effects based on current scientific studies are shown. A large part of thesis is dealing with the chromatographic methods for the separation of phenolic substances including the current trends. The extraction process is also included. The practical part deals with the validation and development of screening HPLC-DAD method for the analysis of monitored phenolic compounds (phloridzin, phloretin, chlorogenic acid, quercitrin, rutin, arbutin, 1,5-dicafeoylquinic acid, and 3,5-dicafeoylquinic acid) in individual parts of fruit trees. The main objective of this thesis is to...
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The use of HPLC technique in the analysis of phenolic compounds in plant material of fruit trees
Adamcová, Anežka ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee) ; Vávra, Radek (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Anežka Adamcová Supervisor: Prof. RNDr. Dalibor Šatínský, Ph.D. Title of the Dissertation Thesis: The use of HPLC technique in the analysis of phenolic compounds in plant material of fruit trees Although fruits are well studied and known for their high content of antioxidants and positive health benefits, the main aim of the presented dissertation thesis consists in the characterization of biological active compounds in individual parts of fruit tree material (leaves, bark, buds, flowers, and wood chips). The theoretical part is focused on fruit trees and the characterization of phenolic compounds. Their properties and the effects based on current scientific studies are shown. A large part of thesis is dealing with the chromatographic methods for the separation of phenolic substances including the current trends. The extraction process is also included. The practical part deals with the validation and development of screening HPLC-DAD method for the analysis of monitored phenolic compounds (phloridzin, phloretin, chlorogenic acid, quercitrin, rutin, arbutin, 1,5-dicafeoylquinic acid, and 3,5-dicafeoylquinic acid) in individual parts of fruit trees. The main objective of this thesis is to...
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Sequential injection chromatography - advanced and two-dimensional separations
Gužiňák, Matej ; Chocholouš, Petr (advisor) ; Šatínský, Dalibor (referee)
Department: Department of analytical chemistry Candidate: Matej Gužiňák Supervisor: doc. PharmDr. Petr Chocholouš, Ph.D. Title of the diploma thesis: Sequential injection chromatography - advanced and two- dimensional separations The subject of this work was the development of two analytical methods intended for separating substances contained in silymarin, their comparison and preparing a template in the Microsoft Excel program to simplify data evaluation. In the first developed method, called classical sequential injection chromatography (1D- SIC), a long Ascentis® Express F5 chromatography column (10 cm x 4.6 mm, 5 µm) with an opti-guard® C18 pre-column (1 mm) was used during analysis. The mobile phase consisted of a mixture of acetonitrile with phosphoric acid solution with pH 2.0 prepared in a ratio of 27:73. The isocratic mode was chosen for the analysis; the total length was 16.3 minutes with a flow rate of 5 μL/s. In the second developed method, called two-dimensional sequential injection chromatography (2D-SIC), a Kinetex® 5 µm EVO C18 column (30 x 3.0 mm) with an opti- guard® C18 pre-column (1 mm) was chosen for the first dimension. In the second dimension, an Ascentis® Express F5 column (30 mm x 4.6 mm, 2.7 µm) was used. The analysis mode was chosen isocratic with a total length of 35.3...
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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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