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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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Aplication of separation methods for determination of biologically active substances
Bílková, Aneta ; Sklenářová, Hana (advisor) ; Česla, Petr (referee) ; Solich, Petr (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: RNDr. Aneta Bílková Supervisor: assoc. prof. PharmDr. Hana Sklenářová, Ph.D. Consultant: assoc. prof. PharmDr. Petr Chocholouš, Ph.D. Title: Application of separation methods for determination of biologically active substances The submitted dissertation thesis presents an annotated set of three publications, focusing on the application of separation methods for the determination of biologically active phenolic substances, pesticide residues in fruits, with regard to the use of modern storage technologies, and the application result - a utility model based again on monitoring the phenolic substances content with respect to different conditions of plant material drying. In the theoretical part, the target analytes are characterized from an analytical point of view, with respect to their physico-chemical properties, stability, antioxidantion activity. It also describes sample preparation methods for the determination of biologically active phenolic substances, selected extraction procedures and an overview of the methods used for the determination of the described substances in plant material. The main part of the dissertation deals with the development, optimization and validation of a rapid...
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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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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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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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Vývoj nové pyruvát-selektivní elektrody pro kontrolu kvality vína
Zelená, Lucie ; Solich, Petr (advisor) ; Sklenářová, Hana (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Lucie Zelená Supervisors: Prof. Maria da Conceição Branco da Silva, Dr. Célia Maria Pinto Gomes Amorim; Department of Analytical chemistry, Faculty of Pharmacy, University of Porto. Prof. RNDr. Petr Solich, CSc; Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague. Title of master's thesis: Development of a new pyruvate-selective electrode for wine control Pyruvate and other organic acids can influence the properties of wines as for example flavor, color, aroma or stability. New fast, low-cost, simple and sensitive methods have been developed for wine quality control. A development of a new selective electrode for potentiometric determination of pyruvate in wine samples was the aim of this work. Sensors based on PVC membrane using 5,10,15,20-Tetraphenyl-21H,23H-porphine manganese (III) chloride as ionophore were under study. Several solvent mediators and lipophilic additives were tested in optimization of response characteristics of sensors. The most interesting response showed membrane with 2-Nitrophenyl phenyl ether as a solvent mediator and Potassium tetrakis(2-chlorophenyl)borate as a lipophilic additive. Sensors with the best characteristics are...
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Stanovení residuí fluorochinolonů v půdách metodou LC-FD
Aufartová, Jana ; Solich, Petr (advisor) ; Nováková, Lucie (referee)
7. Abstract Several pharmaceutics used in human and veterinary medicine could be detected in environment. To these compounds belongs Fluoroqinolones. Our work observed 4 fluoroqinolons (ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin) in soils sample. Fluoroquinolones were determinate by LC-FD. For extraction was used mixture of organic compounds (methanol: acetone; 1:1) and 1.0g of EDTA. Sample was 15 minutes shacked, 15 minutes in ultrasonic bath and 15 minutes of centrifugation. After that organic solution was evaporated by gentle stream of nitrogen in water bath. Rest from evaporation was dissolved in mQ-H2O and clean-up was done. After evaporation after clean-up the rest was dissolved in mobil phase. Mobil phase was H3PO4: MeOH: ACN (920: 70: 10) and flow was 1.4mL/min. Limit of quantification (LOQ) is For OFLO 5mg/L, for NOR is 0.083mg/L, for CIP is 0.116mg/L and for ENRO is 0.125mg/L. Mean recoveries ranged between 75% to 121%, for OFLO, NOR, CIPRO and ENRO. At the beginning we tried also acidic type of extraction. Extraction was made with HCL, H2SO4, H3PO4 and HNO3. In all cases we add EDTA because of interferences with other substances in samples. We find out, that no complex is build between flouroquinolones and EDTA. For clean- up from soil samples is better OASIS column HLB 6cc/200mg....
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Sledování norfloxacinu, ciprofloxacinu a enrofloxacinu pomocí HPLC-FD ve vzorcích odpadních vod a jejich vliv na životní prostředí
Spurná, Marie ; Solich, Petr (advisor) ; Chocholouš, Petr (referee)
8 Abstract Fluoroquinolones (FQs) are used for therapy and prophylaxis of human and animal diseases and they are also used as growth promoters of animals. The usage of antibiotic is in connection with development of antibiotic resistance among bacterial populations. Since swine production industry is considered to be a relevant source of antibiotic resistant bacteria, measures to control the use of antimicrobial agents in animal husbandry have been adopted in recent years (1). The presence of FQs in wastewater from swine farms can introduce antibiotics in surface waters through agricultural runoff. FQs are rather resistant to microbial degradation and these compounds may be persisting within environmental waters because of their sorption properties, favouring the accumulation in sewage sludge, manure and soil (2). To trace the sources and ways of contamination, and evaluate the environmental impact of an outdoor swine production system, the occurrence norfloxacin (NOR), ciprofloxacin (CIP) and enrofloxacin (ENRO) residues were evaluated in wastewater and surface water samples. A LC-FD method based on the application of monolithic column (Chromolith Performance RP-18e (100 x 4.6 mm) successfully developed in previous studies (3,4,5) was applied. FQs were isocratically eluted using a mobile phase consisting...
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Using of sequential injection chromatography method for separation and determination of salicylic acid and triamcinolone acetonide in pharmaceutical preparation Triamcinolon-IVAX
Holík, Pavel ; Šatínský, Dalibor (advisor) ; Solich, Petr (referee)
Using of sequential injection chromatography method for separation and determination of salicylic acid and triamcinolone acetonide in pharmaceutical preparation Triamcinolon-IVAX Pavel Holík Abstract A novel and fast simultaneous determination of triamcinolone acetonide (TCA) and salicylic acid (SA) in topical pharmaceutical formulations by sequential injection chromatography (SIC) as an alternative to classical high performance liquid chromatography (HPLC) has been developed. A recently introduced Onyx™ monolithic C18 (50 mm × 4,6 mm, Phenomenex® ) with 5 mm monolithic precolumn were used for the first time for creating sequential injection chromatography system based on a FIAlab® 3000 with a six-port selection valve and 5,0 ml syringe pump in study. The mobile phase used was acetonitrile/water (35:65, v/v), pH 3.3 adjusted with acetic acid at flow rate 15 µl.s-1 . UV detection provided by fibre-optic DAD detector was set up at 240 nm. Propylparaben was chosen as suitable internal standard (IS). There is only simple pre-adjustment of the sample of topical solution (dilution with mobile phase) so the analysis is not uselessly elongated. Parameters of the method showed good linearity in wide range, correlation coefficient >0,999; system precision (relative standard deviation, R.S.D.) in the range 0,45-1,95%...
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Development of Automated SIA System for Parallel Determination of Target Anions
Dundová, Aneta ; Solich, Petr (advisor) ; Šatínský, Dalibor (referee)
This rigorosis thesis is divided into two parts, which are closely related. The first part deals with optimization of conditions for the determination of dissolved silicates using sequential injection analysis adjusted in accordance with applicable ISO standards for the FIA method, the second, main part of work deals with the development of the automated SIA system for the parallel determination of selected anions in the commercial SIA system. CSN EN ISO 16 264 describing FIA metodology suitable for determination of dissolved silicates with spectrophotometric detection was based on the reaction of a sample containing dissolved silicates with the reagent (acid solution of heptamolybdate), which reacts with the silicates and phosphates to form acid molybdato - silicate and molybdatophosphate, which is then decomposed by oxalic acid. Molybdatosilicate acid is reduced by acidic solution of stannous chloride to the resulting product of the reaction - molybdenum blue - that was measured at 710nm. In the experimental work transfer of the FIA method to the determination in the sequential injection system in compliance with the calibration ranges listed in the ISO standard was carried out. Calibration curves showed linearity in the range c = 0.2 to 2.0 mg /l and c = 2.0 to 20.0 mg /l with a correlation...
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