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Vývoj optického sensoru pro salicylát
Soukupová, Marie ; Matysová, Ludmila (advisor) ; Sklenářová, Hana (referee)
We dealt with the development of optical sensor for salicylate. Sensing layer of sensor was based on metalloporphyrins. Metalloporphyrins embody great optical features. Metalloporphyrins are commonly employed as ionophores in ion-selective electrodes (ISEs). Observations from work with ISEs are applied to optical sensors. At first, membrane was constructed, based on tetraphenylporphyrin copper(II) (Cu(TPP)) and it did not show significant sensitivity towards salicylate. Further there were membranes created from tetraphenylporphyrin manganese(III)chloride (Mn(TPP)) and gallium(III)phthalocyanine chloride (Ga(PC)). Reactivity of Mn(TPP) was comparable with reactivity of Cu(TPP). Membrane from Ga(PC) displayed considerable reactivity and sensitivity towards salicylate. Later the membrane's capability was tested to detect valproate. We discovered that the limit of detection for valproate is much lower than for salicylate. Due to great reactivity and variability in membrane response in spectrophotometric assay we were not able to set the working conditions for application to flow system and to dissolution as well. Ga(PC) has thus very good potential in use for detection of valproate. Valproate is one of the most used antiepileptic drugs.
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Using of macrocyclic glycopeptide sorbents in a chiral analysis of beta-blockers by method HPLC
Zdarsová, Ivana ; Nováková, Lucie (advisor) ; Matysová, Ludmila (referee)
Using of macrocyclic glycopeptide sorbents in a chiral analysis of beta-blockers by method HPLC Ivana Zdarsová Abstract The aim of this work was to introduce with possibilities of macrocyclic glycopeptides stationary phases (vancomycin and teicoplanin) to separation from chosen β-blockers (atenolol, pindolol and propranolol) by HPLC method with diode array detection. The next aim was to arrange optimal conditions (column, composition of mibole phase, temperature and flow of mobile phase) for enantioseparation. Vancomycin and teicoplanin sorbent were tested by using the polar-ionic mode and reverse mode. The influence of concentration of acid and base in an organic solvent, the temperature and composition of the organic solvent was tested in the polar-ionic mode. The influence of pH aqueous part, the rate of organic and aqueous components of the mobile phase was tested in the reverse mode. There was no separation of enantiomers from β-blockers at all, when was used reverse mode in CHIROBIOTIC V and CHIROBIOTIC T. There was no enantiseparation of atenolol in the polar-ionic mode in CHIROBIOTIC T with a resolution above 1,5. There was enantioseparation of pindolol with a resolution above 1,5 when two mobile phase was used and enantioseparation of propranolol with resolution above 1,5 was when all mobile phase...
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The Usage of HPLC in Pharmaceutical Analysis
Krivda, Anton ; Matysová, Ludmila (advisor) ; Nováková, Lucie (referee)
Title: The usage of HPLC in pharmaceutical analysis Name: Anton Krivda This labour deals with determination and validation of method suitable for qualitative and quantitative analysis of dimetindeni maleas in Fenistil® gel trough the use of high performance liquid chromatography with UV detection. There were two differential analytical columns tested (C18 and ZICTM column). Acceptable outcomes were got with these chromatographic conditions: wavelength λ = 258 nm. analytical column: SeQuant ZICTM Column(50 x 2.1 mm; 5 μm) compound of mobile phase: acetonitrile : aqeous solution of acetic acid (25 mM) and ammonium acetate (2,5 mM), (87,5:12,5) flow rate fm = 0,3 ml/min internal standard: diltiazem hydrochloride Recovery, effectivity of column, assymetry and resolution of chromatographic peaks were tested in validation tehse method. Each of them reposed in licenced range.
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Development and validation of HPLC method for separation and determination of active substances in pharmaceutical preparation Valetol
Ullrichová, Jana ; Šatínský, Dalibor (advisor) ; Matysová, Ludmila (referee)
Development and validation of HPLC method for separation and determination of active substances in pharmaceutical preparation Valetol Jana Ullrichová Abstract A method for the determination of paracetamol, propyphenazone and caffeine by the high- performance liquid chromatographic method with ultraviolet detection has been developed and validated. The analysis was performed at the room temperature in an isocratic mode on the reversed phase ODS Hypersil 5 µm C-18 column (250x4,6mm). A mobile phase (water : 2-propanol : diethylamine : methanol (50 + 15 + 3 + 32) adjusted to pH 7.5 by means of phosphoric acid) was suitable for the separation and the determination of paracetamol, caffeine and propyphenazone. UV detection was applied at 273 nm. Injected volume was 5 µl, flow rate 0,5 ml.min-1 . The developed method is sensitive and selective and can be applied for the routine studies of pharmaceuticals in the tablet form.
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Development and validation of HPLC methods for analysis of pharmaceutical formulations
Matysová, Ludmila ; Solich, Petr (advisor) ; Karlíček, Rolf (referee) ; Nobilis, Milan (referee)
7. Summary Development and validation of HPLC methods The doctoral thesis concerns with development of HPLC methods for analysis of pharmaceutical formulations, which meet all requirements for suitability, precision and reliability. Documentation of these parameters is called validation. At first theoretical principles of chromatography are described in this work, with the emphasis to liquid chromatography, included HPLC. The instrumentation in HPLC is described, mentioning the new trends in stationary phase's development - for example monolithic columns, zirkonia stationary phase, HILIC and sub-2-microns phases. In the other part UPLC system, one of the new trends in liquid chromatography development is discussed. Next part deals with the development of HPLC methods for analysis of pharmaceutics and is followed by chapter, in which analysis of pharmaceutical formulations is described, included preparation of the samples before analysis, stability monitoring and further the analysis of impurities. The last, relatively large chapter is dealing with the validation of analytical methods. Several institutions are concerned with validation requirements. They issue recommendation and/or guidelines, which are cogent for this process. In the Czech Republic there exists State Institute for Drug Control (SUKL -...
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Dispersive Solid-Phase Extraction for the Analysis of Chosen Substances in Zingiber officinale
Urbanová, Martina ; Chocholoušová Havlíková, Lucie (advisor) ; Matysová, Ludmila (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Urbanová Consultant: PharmDr. Lucie Chocholoušová Havlíková, Ph.D. Thesis Title: Dispersive Solid-Phase Extraction for the Analysis of Chosen Substances in Zingiber officinale The thesis was focused on the development of optimal extraction method for the analysis of chosen substances contained in Zingiber officinale. Some representative samples containing extracts of Zingiber officinale were chosen. This method was based on the diploma thesis of Martina Urbanová [1]. To get a higher preconcentration factor, dispersive solid-phase extraction (dSPE) was tested for the sample pretreatment. Then, a method of supported liquid extraction (SLE) was examined as another methodology for the sample preparation. Chosen substances, 6-gingerol, 8-gingerol, 6-shogaol and 10-gingerol, were found in almost all samples. Among syrups, the largest amount of substances was contained in the Kitl syrup (preparation with cold water). Among teas, the highest number of substances was contained in Fruit-herbal tea flavored with ginger and lemon. 6-Shogaol was not found in rhizome samples, however, it has been found in the samples of teas and syrups. During the optimization of this method, various...
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