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Determination of pindolol by sequential injection analysis with chemiluminescence detection
Havelková, Jana ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
The oxidation of the drug pindolol, [1-(indol-4-yloxy)-3-(isopropylamino)-2-propanol (I)] by permanganate in the medium of aqueous H2SO4 is accompanied by the emission of chemiluminescence (CL) radiation. The CL signal is enhanced by hexametaphosphate. This CL reaction was used for devising automated sequential injection analysis (SIA) assay of I in pharmaceutical preparations. The PC-controlled SIA setup consisted of a Cavro XL 3000 2.5- ml syringe pump, Vici-Valco 10-port selection valve and Spectra-Physics FS970 flow- through fluorescence detector equipped with a lab-made CL detection module. The net CL signal of I increased by a factor of 4.4 (compared to purely aqueous test solution of I injected) if the test solution contained 80% (v/v) of methanol. Optimal order, concentrations and volumes of aspirated zones of reactants were: 43l of 80mM Na hexametaphosphate, 30 l of I in 80% (v/v) methanol, 28 l of 2M H2SO4 and 1 l of 5mM KMnO4. Calibration curve relating the intensity of CL (peak height) to the concentration of I was linear in the range 1 - 10 M I; the limit of detection (S/N = 3) was 0.15 M I. The sample throughput was 90 h-1 . The repeatability of the peak heights was characterized by RSD 1.8% for 30 replicate injections of 8 M I. The SIA-CL method was used for the assay of I in...
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Analysis of Calcium Pantothenat, Methylparaben and Propylparaben by Micellar Electrokinetic Chromatography
Balcar, Josef ; Pospíšilová, Marie (advisor) ; Polášek, Miroslav (referee)
1. ABSTRACT 1.1. ANALYSIS OF CALCIUM PANTOTHENAT, METHYLPARABEN AND PROPYLPARABEN BY MICELLAR ELECTROKINETIC CHROMATOGRAPHY Josef Balcar Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Analytical Chemistry, Heyrovského 1203, Hradec Králové In this study, a new micellar electrokinetic chromatography (MEKC) has been developed for the simultaneous analysis of calcium pantothenat, methylparaben and propylparaben. Separations were carried out in a fused silica capillary (7,5 cm × 75 μm i.d.) at 20 kV with UV detection at 200 nm. The optimal background electrolyte was 40 mM tricine buffer (pH* 8.2) containing 50 mM sodium dodecyl sulfate as a surfactant and 20 % (V/V) methanol. Rectilinear calibration ranges were 50.0 - 500.0 mg/100ml for calcium pantothenat, 2.0 - 20.0 mg/100ml for methylparaben and 0.5 - 5.0 mg/100ml for propylparaben. The validated MEKC method was applied to the determination of the analytes in a pharmaceutical preparation. The total analysis time was <3 min.
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Determination of bopindolol by the technique of sequential injection analysis with chemiluminescence detection
Holá, Petra ; Polášek, Miroslav (advisor) ; Šatínský, Dalibor (referee)
The oxidation of bopindolol [ 4-(2-benzoyloxy-3-tert-butylaminopropyl)-2-methylindole (I)], by permanganate in the medium of aqueous H2SO4 is accompanied by the emission of chemiluminescence (CL) radiation. The CL signal is enhanced by hexametaphosphate. This CL reaction was used for devising automated sequential injection analysis (SIA) assay of I in pharmaceutical preparations. The PC-controlled SIA setup consisted of a Cavro XL 3000 2.5- ml syringe pump, Vici-Valco 10-port selection valve and Spectra-Physics FS970 flow- through fluorescence detector equipped with a lab-made CL detection module. The net CL signal of I increased by a factor of 3 (compared to purely aqueous test solution of I injected) if the test solution contained 60% (v/v) of methanol. Optimal order, concentrations and volumes of aspirated zones of reactants were: 61l of 80mM Na hexametaphosphate, 60 l of I in 60% (v/v) methanol, 40 l of 30mM H2SO4 and 9 l of 0.5mM KMnO4. Calibration curve relating the intensity of CL (peak height) to the concentration of I was linear in the range 1 - 8 M I; the limit of detection (S/N = 3) was 0.2 M I. The sample throughput was 100 h-1 . The repeatability of the peak heights was characterised by RSD 1.8% for 15 replicate injections of 2 M I. The SIA-CL method was used for the assay of I...
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Chemiluminescence determination of thioridazinem, promethazine and levomepromazine using the flow injection analysis
Kolouchová, Gabriela ; Dolejšová, Jana (advisor) ; Polášek, Miroslav (referee)
1. SOUHRN V literatuře jsem vyhledala články týkající se různých způsobů stanovení fenothiazinových derivátů ( thioridazinu, promethazinu a levomepromazinu ) a práce zabývající se využitím FIA metody s chemiluminiscenční a fluorimetrickou detekcí ve farmaceutické analýze. Otestovala jsem systém FIA řízený počítačem a nastavila jsem vhodné parametry přístroje ( doba dávkování, rychlost čerpání roztoků do systému, časové parametry ), které jsem zachovávala po celou dobu měření konstantní. Určila jsem optimální složení nosného proudu a otestovala vliv některých látek na intenzitu chemiluminiscence. Největší vliv na intenzitu chemiluminiscence byl prokázán u polyfosfátu sodného. Ten jsem použila při proměřování kalibrační závislosti. Za optimalizovaných podmínek jsem proměřila kalibrační křivky thioridazinu, promethazinu a levomepromazinu bez a s přídavkem PFS o desetkrát nižší koncentraci thioridazinu, promethazinu a levomepromazinu. Tu jsem poté použila k odečtení koncentrací léčiv ve farmaceutických přípravcích. Zjištění obsahu levomepromazinu v přípravku Tisercin® inj. jsem nemohla FIA metodou uskutečnit. Intenzitu chemiluminiscence zvyšuje obsažená antioxidační přísada acidum ascorbicum. Podniková norma nebyla k dispozici. Obsah thioridazinu v přípravku Thioridazin ® 25 mg, tbl. obd. a obsah promethazinu v...
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New mass spectrometric methods for trace gas analysis of human breath.
Brůhová Michalčíková, Regina ; Španěl, Patrik (advisor) ; Polášek, Miroslav (referee) ; Tichý, Milan (referee)
This dissertation thesis summarizes results of experiments that have been carried out during my PhD studies related to the new mass spectrometric methods for trace gas analysis of human breath. The thesis is divided into the theoretical and experimental part. The chapter at the beginning of this dissertation summarizes the current research in the area of breath analysis. It is describing the common breath metabolites, benefits and challenges of the method for therapeutic monitoring and clinical diagnosis and current applications. The next chapter of the theoretical introduction describes the techniques suitable for this area of research, with a special emphasis on mass-spectrometric techniques (in particular the selected ion flow tube mass spectrometry, SIFT-MS, method that allows accurate quantification of trace gases and vapours in humid air/human breath). All these parts are elaborated via the scientific literature review. The following chapters are then directly related to my own research and describes the conducted experiment, including the results obtained. This experimental part "Results and Discussion" is divided to the individual subsections, which are conceived as the commentaries to the enclosed research papers published in peer reviewed journals. The first is the detailed step by step...
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Determination of selected impurities in quaternary ammonium compounds with potential antibacterial effect by capillary zone electrophoresis
Prskavcová, Pavla ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
In this study, capillary zone electrophoresis with UV detection was developed for separation and determination of impurities pyridine and isoquinoline in quaternary ammonium compounds. The analysis was performed in a fused silica capillary at 20 kV and 25 řC with UV detection at 210 nm and 254 nm. The total length of the capillary was 58 cm, the effective length was 49,5 cm and its inner diameter was 75 µm. The injection was carried out for 6 seconds and under pressure of 50 mbar. The analysis took less than 5 minutes. The optimal background electrolyte consisted of 70 mM acetic acid with 5% (v/v) of methanol. pH was adjusted to 4,7 with sodium hydroxide. As internal standard was chosen imidazole. The calibration graphs were linear for both pyridine (0,1 - 10,4 µg/ml; r2 = 0,9988) and isoquinoline (0,1 - 9,98 µg/ml; r2 = 0,9972). The limits of detection were 0,06 µg/ml for pyridine and 0,02 µg/ml for isoquinoline. The optimized method has been used to determine the content of pyridine and isoquinoline as impurities in samples of quaternary ammonium compounds.
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Electrophoretic determination of selected muscle relaxants using contactless conductivity detection
Lužová, Veronika ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
A novel capillary electrophoretic method for the separation of pancuronium (PM) and vecuronium (VM) ions utilizing capacitively coupled contactless conductivity detection (C4 D) was devised and validated. The separation was carried out in bare fused-silica capillaries (50 µm i.d., 75/45 cm) at 25 řC. Optimal background electrolyte was 50 mM borate buffer of pH 9.5 containing 12.5 mg/ml of hydoxypropyl-γ-cyclodextrine; (phenyltrimethylammonium iodide was used as internal standard). The samples were injected hydrodynamically at 1000 mbar for 3 s. The separation was performed at +30 kV. Under such conditions the PM and VM were base-line resolved and the separation took < 4 min. Calibration curves were linear for both PM bromide and VM bromide in the range 25-250 μg/ml with r > 0.9968. The limits of detection were 7 and 6 μg/ml for PM bromide and VM bromide, respectively. The accuracy tested by recovery experiment at three concentration levels of added PM bromide and VM bromide was satisfactory (95.7-102.7 %, n=3, with RSD < 2.61 %). The method was successfully applied to the assay of PM bromide and VM bromide in commercial injection solutions.
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Determination of 6-sulfatoxymelatonin by capillary electrophoresis
Klimánková, Karla ; Jezberová, Michaela (advisor) ; Polášek, Miroslav (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate Mgr. Karla Klimánková Consultant RNDr. Michaela Hamerníková, Ph.D. Title of Thesis Determination of 6-sulfatoxymelatonine by Capillary Electrophoresis The submited thesis deals with a development of a method for determination of 6-sulfatoxymelatonine for purposes of the gerontological research. Parameters of the electrophoretic determination were optimized, i. e.: composition of the base electrolyte, its pH, voltage, time of injection. Then folloving validation parameters were determined: linearity, repeatability, reproducibility of migration times and limit of detection. The obtained results confirm the applicability of the method for the given purpose.
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