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Employment of gas chromatography in the field of drug control I.
Holeksa, Miroslav ; Kučera, Radim (advisor) ; Sochor, Jaroslav (referee)
1. ABSTRACT Ethylenoxide is a volatile gas, used for medical instrument sterilization in hospital, which can not stand heat sterilisation. Ethylenoxid is a cancerogenic and a mutagenic substance and for that reason there are put high demands on residual content in instruments after sterilization. Optimalization of chromatographic conditions was realized in this diploma thesis. Gas chromatograph Shimadzu GC-2010 and PC with chromatographic software GC solution Analysis Ver.:2.21 were used. Restek Rtx®-1 (100% dimethylpolysiloxan), 30 m, 0,32 mm; 1 µm column was used. Carrier-gas (He) flow rate was 1,05 ml/min. Particular conditions for chromatographic determination were optimalised in succesive steps (suitable solvent, thermostating time period and temperature, gas syringe temperature and sample volume). Following conditions of headspace analysis were choosen. Headspace vial thermostating time 30 minutes, temperature 90řC, gas syringe temperature 60řC and DMSO as a solvent. Calibration curve was construed to determinate ethylenoxide content. Its equation is y = 1620x - 6,627 (R2 = 0,999). Before analysis, particular ethylenglycol samples were appropriately modified and injected onto column. Content of ethylenoxid, determined in three samples by calibration curve, was matched to the limit of ethylenoxide...
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HPLC Analysis of Dexamethasone in Topical Preparations
Janurová, Catherine ; Sochor, Jaroslav (advisor) ; Kastner, Petr (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Mgr. Catherine Janurová Consultant: Doc. RNDr. Jaroslav Sochor, CSc. Title of Thesis: HPLC analysis of dexamethasone in topical preparations The subject of this paper is the HPLC evaluation of dexamethasone in topical preparations. Dexamethasone was analysed by the use of a C-18 column, a water: acetonitrile (40:60) mobile phase, flow rate of 1,0 ml/min and a UV detector set at 239 nm. An internal standard was used for quantitative determination. A calibration curve was constructed and verified, by means of which the concentration of dexamethasone in selected topical preparations was determined. A standard calibration curve was constructed and the determination of dexamethasone in these topical preparations was tested. Considering the obtained results, the application of a calibration curve in the relevant ointment base from which dexamethasone is quantified, is preferable. A rigorous evaluation for the generalisation of this conclusion is required. The above developed method was validated and a test for its efficacy was evaluated. By verifying the validation parameters: precision, accuracy, selectiveness, linearity, detection limit, quantitative limit and...
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HPLC evaluation of select drugs V.
Kašková, Jana ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Jana Kašková Consultant: RNDr. Milan Mokrý, CSc. Title of Thesis: HPLC evaluation of some drugs V. This thesis is about looking for the optimal conditions for simultaneous HPLC analysis in combined tablets of amlodipin and atorvastatin with subsequent determination of their content. As the most suitable stacionary phase was chosen chromatographic column 125x4 mm I. D. contains Nucleosil 120-5 C 18, Macherey-Nagel, and the mobile phase formed by mixture of acetonitrile - disodium hydrogen phosphate dodecahydrate solution (0,025 mol/l) in the ratio 55:45, acidified with phosporic acid at pH 4,4 at a flow rate of 1,0 ml/min and temperature 25řC. Propylparaben was used as the most suitable internal standard. The detection was performed at 210 nm using an UV-VIS detector. At the determination of content of medicaments in tablets was found that used compounds were eluted in following order: propylparaben, atorvastatin and amlodipine besylate.
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Analytical determination of active compounds by liquid chromatography.
Janurová, Catherine ; Sochor, Jaroslav (advisor) ; Kastner, Petr (referee)
Analytical determination of active compounds by liquid chromatography Diploma Thesis Catherine Janurová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové This paper deals with the HPLC evaluation of dexamethasone in ointment base. Dexamethasone was analysed by the use of a C-18 column, a water: acetonitrile (40:60) mobile phase, flow rate of 0,6 ml/min and a UV detector set at 239 nm. An internal standard was used for quantitative determination. Acetonitrile was shown to be the best solvent for the isolation of dexamethasone from the ointment base. A calibration curve was constructed and verified, by means of which the concentration of dexamethasone in ointment was determined. The elaborated method was validated. Validation parameters: precision, accuracy, selectiveness, linearity, detection limit, quantitative limit and robustness were evaluated.
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HPLC evaluation of selected drugs II
Vyroubal, Petr ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
HPLC evaluation of selected drugs II. THESIS Petr Vyroubal Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this thesis was validated method for simultaneous HPLC analysis of paracetamol and tramadol in combined tablet. As stationary phase the chromatographic column Discovery HS F5, 5 µm, 150×3 mm I.D. made by Supelco was used. Mobile phase was formed by mixture of acetonitrile : ammonium acetate solution 0.005 mol/l, acidified with acetic acid at pH 3.2 in the ratio 20:80 (v/v). A flow rate was 1.0 ml/min. Acetylsalicylic acid was used as an internal standard. The detection was performed at λ = 270 nm using an UV detector. The substances were eluted in following order: paracetamol, acetylsalicylic acid and tramadol. The method was validated for linearity (paracetamol R = 0.9996; tramadol R = 0.9998), precision (paracetamol RSD = 0.31 %; tramadol RSD = 0.70 %), accuracy (paracetamol recovery = 99.49 %; tramadol recovery = 98.90 %) and robustness.
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Analytical evaluation of drugs by liquid chromatography VI
Rosecký, Jan ; Sochor, Jaroslav (advisor) ; Mokrý, Milan (referee)
Analytical evaluation of drugs by liquid chromatography VI Degree paper Jan Rosecký Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové The aim of this degree paper was to optimize conditions for the determination of 6-aminocaproic acid, hydrolytic degradation product of accelerant of transdermal penetration transkarbam 12, using high-performance liquid chromatography (HPLC) and subsequently to validate this method. 3,5-dinitrobenzoyl chloride was used before HPLC analysis for derivatization of 6-aminocaproic acid. Analysis of derivatized acid was performed on Separon SGX C-18 analytical column (150 x 3mm I.D, 5µm). The gradient elution was used for the separation. The mobile phase was consisted of acetonitrile and sodium acetate buffer pH 4,5 and the flow rate was 1 ml/min. 20 µl sample volumes were injected into the chromatographic system. Wavelength used for the detection was 230 nm. The method of internal standard was used for quantitative evaluation of derivatized 6-aminocaproic acid and 7-aminocaprylic acid was chosen as the most suitable internal standard. After the development of the method, these validation parametres were evaluated: precision, accuracy, linearity, selectivity,...
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Analytical determination of active compounds by liquid chromatography II
Raška, Martin ; Sochor, Jaroslav (advisor) ; Kovaříková, Petra (referee)
ANALYTICAL DETERMINATION OF ACTIVE COMPOUNDS BY LIQUID CHROMATOGRAPHY II. The Preliminary Study of SPME Master's Thesis Martin Raška Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové This thesis deals with the issue of analytical determination of active compounds by liquid chromatography. It's specifically focused on determination of benzodiazepines in biological material by using solid-phase microextraction (SPME) and high performance liquid chromatography (HPLC). HPLC is one of the most important chromatographic methods today. Its main advantages are sensitivity, selectivity and speed of separation and creation of reproducible record. SPME can be described as a simple and effective sample preparation technique integrating sorption, desorption and concentration of an analyte. This technique is solvent-free and requires no use of a complicated apparatus. Its basic principle is the exposure of liquid or fluid sample to a small amount of extraction phase. The following chromatographic conditions were proved to be optimal. Methanol:water (80:20) was used as a mobile phase with pH value adjusted to 7.5, flow rate was 0.8 ml/min and detection wavelength was 254 nm. Polydimethylsiloxane fiber...
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HPLC analysis of drugs III
Blažková, Petra ; Sochor, Jaroslav (advisor) ; Mokrý, Milan (referee)
ANALYTICAL EVALUATION OF ACTIVE SUBSTANCE BY LIQUID CHROMATOGRAPHY II. Diploma thesis Petra Blažková Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové The subject of this diploma thesis is a determination of active substances by liquid chromatography. In particular it deals with an evaluation of phenobarbital in biological matrix. Solid phase microextraction (SPME) and high performance liquid chromatography (HPLC) with UV detector (218 nm) and reversed phase C18 comlumn were used. The mobile phase consisted of methanol and phosphate buffer in a ratio of 50:50. The flow rate was set to 0,4 ml/min. 20 µl of sample solution was injected on the chromatographic column. Phenobarbital was dissolved in a mixture of methanol and buffer in a ratio of 80:20. For the SPME extraction from water solution was used carbowax/TPR fibre. The analyte was desorbed into methanol. The extraction time was 20 minutes. Phenobarbital extraction from rabbit plasma was performed in the same way, but PDMS/DVB fibre instead of carbowax/TPR fibre was used. Phenobarbital in rabbit plasma was quantified by means of calibration curve.
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