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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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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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Modern chromatographic techniques in food contamination analysis
Lhotská, Ivona ; Šatínský, Dalibor (advisor) ; Karlíček, Rolf (referee) ; Malíř, František (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Ivona Lhotská Supervisor doc. RNDr. Dalibor Šatínský, Ph.D. Title of Doctoral Thesis Modern chromatographic techniques in food contamination analysis A compilation of seven publications dealing with chromatographic methods for determination of food contamination (particularly mycotoxins and artificial food colorants) is presented in dissertation thesis. All methods were fully validated, complying with the requirements and applied for real samples analysis. The first part describes the methods for mycotoxins determination based on on-line solid phase extraction (SPE) utilizing column-switching system. Reversed phase columns packed with superficially porous particles were chosen for both extraction and separation step during optimization of on-line SPE-HPLC method for ochratoxin A and citrinin determination in beer. In following work, determination of patulin in juices and zearalenone in beer, more selective molecularly imprinted polymers (MIP) were used for on-line extraction. Due to challenging optimization of on-line MIP SPE, the methods were compared to off-line MIP extraction and on-line extraction using conventional C18 phase to confirm the selectivity. The employed commercial MIP...
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Column switching chromatography for mycotoxines determination in Czech beer samples
Lhotská, Ivona ; Ramos, María Carolina Fernández (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Ivona Lhotská Supervisor, consultant: María Carolina Fernández Ramos, Ph.D, Doc. RNDr. Dalibor Šatínský, Ph.D. Title of Diploma Thesis: Column switching chromatography for mycotoxines determination in Czech beer samples A new fast and sensitive method of high performance liquid chromatography for simultaneous determination of mycotoxins ochratoxin A and citrinin using column- switching system for on-line sample pretreatment was developed. 100 µl of beer was injected directly into the chromatographic system. Isolation of analytes was performed on guard column Ascentis Express RP-C18 (5 x 4.6 mm, 2.7 µm) washing out with methanol - water solution of acetic acid 0.5% (30:70, v/v), at a flow rate 2 ml/min; time of valve switch was set on 2 minutes. The separation was performed on Ascentis Express Phenyl-Hexyl column (100 x 4.6 mm, 2.7 µm) with mobile phase of composition acetonitril - water solution of acetic acid 0.5% at a flow rate 1 ml/min. A gradient was increasing up to 75:25 linearly in time 3 - 5.5 min. The temperature 50řC was set up for column separation. Wavelengths of fluorimetric detection were set at Ex 335 nm, Em 497 nm. Analysis of one sample including on-line pretreatment was...
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Development of HPLC method for determination of selected phenolic acids and flavonoids in Tokaj wines
Moravcová, Pavlína ; Šatínský, Dalibor (advisor) ; Lhotská, Ivona (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical chemistry Candidate: Bc. Pavlína Moravcová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Development of HPLC method for determination of selected phenolic acids and flavonoids in Tokaj wines The aim of this diploma thesis was to develop and optimize HPLC method for simultaneous determination of 15 phenolic compounds, protocatechic acid, fertaric, coffee, p-hydroxybenzoic, syringic, gallic, p-coumaric, ferulic, chlorogenic, caftaric, 2-hydroxy-4-methoxybenzoic , polydatin, resveratrol, catechin hydrate and epicatechin in Tokaj wines. The quantity and content of selected phenolic compounds was analyzed in 25 samples of Tokaj wines, which come from vineyards from the Slovak part of Tokaj wine region. The work was also focused on the description of the specific characteristics of this unique area, the unique method of Tokaj wine production, its chemical composition, and namely the spectrum of phenolic substances. Analysis of selected phenolic compounds was performed using an Ascentis® Express F5 column (150 x 4.6 mm; 5 µm) using a mobile phase consisting of 0.1% phosphoric acid and acetonitrile in gradient elution. The substances were analyzed at 30 řC and flow rate of 1 ml/min and detected...
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Development of UHPLC-MS/MS method for analysis of selected antivirotics in HILIC and RP mode
Fical, Luboš ; Nováková, Lucie (advisor) ; Lhotská, Ivona (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Luboš Fical Supervisor: Prof. PharmDr. Lucie Nováková, Ph.D. Title of the diploma thesis: Development of UHPLC-MS/MS method for analysis of selected antivirotics in HILIC and RP mode The goal of this diploma thesis is development and optimization of methods for analysis of selected antivirals and comparison of suitability of RP and HILIC modes for this application. Targeted antivirals are used in treatment of HIV and hepatitis B and/or C. LC analyses were carried out on the ACQUITY UPLC I-Class PLUS system with triple quadrupole MS detector. Initially MS/MS method was optimized. In RP mode total of 6 stationary phases (BEH Shield RP18, BEH Phenyl, BEH C18, CSH Fluoro-phenyl, CSH Phenyl-hexyl, and CSH C18) and 4 mobile phases (ACN in gradient elution with aqueous component: formic acid, acetic acid, ammonium formate pH 3, ammonium acetate pH 9) were tested. Separation conditions were as follow: temperature 40řC, flow rate 0.3 mL/min, gradient elution from 5 % ACN to 98 % ACN within 5 minutes with isocratic step at the end of analysis. In HILIC mode 10 stationary phases (BEH Amide, BEH HILIC, Cortecs HILIC, Ascentis Express HILIC, Ascentis Express OH5, Syncronis HILIC, Kinetex HILIC, Luna HILIC,...
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Development of UHPLC-MS/MS method for analysis of selected antivirotics in HILIC and RP mode
Fical, Luboš ; Nováková, Lucie (advisor) ; Lhotská, Ivona (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Luboš Fical Supervisor: Prof. PharmDr. Lucie Nováková, Ph.D. Title of the diploma thesis: Development of UHPLC-MS/MS method for analysis of selected antivirotics in HILIC and RP mode The goal of this diploma thesis is development and optimization of methods for analysis of selected antivirals and comparison of suitability of RP and HILIC modes for this application. Targeted antivirals are used in treatment of HIV and hepatitis B and/or C. LC analyses were carried out on the ACQUITY UPLC I-Class PLUS system with triple quadrupole MS detector. Initially MS/MS method was optimized. In RP mode total of 6 stationary phases (BEH Shield RP18, BEH Phenyl, BEH C18, CSH Fluoro-phenyl, CSH Phenyl-hexyl, and CSH C18) and 4 mobile phases (ACN in gradient elution with aqueous component: formic acid, acetic acid, ammonium formate pH 3, ammonium acetate pH 9) were tested. Separation conditions were as follow: temperature 40řC, flow rate 0.3 mL/min, gradient elution from 5 % ACN to 98 % ACN within 5 minutes with isocratic step at the end of analysis. In HILIC mode 10 stationary phases (BEH Amide, BEH HILIC, Cortecs HILIC, Ascentis Express HILIC, Ascentis Express OH5, Syncronis HILIC, Kinetex HILIC, Luna HILIC,...
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Modern chromatographic techniques in food contamination analysis
Lhotská, Ivona ; Šatínský, Dalibor (advisor) ; Karlíček, Rolf (referee) ; Malíř, František (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Ivona Lhotská Supervisor doc. RNDr. Dalibor Šatínský, Ph.D. Title of Doctoral Thesis Modern chromatographic techniques in food contamination analysis A compilation of seven publications dealing with chromatographic methods for determination of food contamination (particularly mycotoxins and artificial food colorants) is presented in dissertation thesis. All methods were fully validated, complying with the requirements and applied for real samples analysis. The first part describes the methods for mycotoxins determination based on on-line solid phase extraction (SPE) utilizing column-switching system. Reversed phase columns packed with superficially porous particles were chosen for both extraction and separation step during optimization of on-line SPE-HPLC method for ochratoxin A and citrinin determination in beer. In following work, determination of patulin in juices and zearalenone in beer, more selective molecularly imprinted polymers (MIP) were used for on-line extraction. Due to challenging optimization of on-line MIP SPE, the methods were compared to off-line MIP extraction and on-line extraction using conventional C18 phase to confirm the selectivity. The employed commercial MIP...
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