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HPLC Analysis of Vitamines Soluble in Water Using Electrochemical Detector
Jesenský, Ivan ; Kastner, Petr (advisor) ; Mokrý, Milan (referee)
High performacne liquid chromatography is valued analytical method, which is one of the most frequently used in pharmacy. Biotine is at water soluble vitamin, which is an important element of various enzyme, stuff necessary in metabolism. It part take on metabolism of sugar, fat and protein. It occur in several sort of food, especially in roast, peanut butter, egg yolk, carrot, peas, soya, wheat gemmule and oaten flake. This work deals with optimalization chromatographic condition on determination of biotine. Its target is to find optimal mobile phase, near which give out best separation biotine from others element in solution, to find internal standard and form hydrodynamic voltamogramms, individual at water soluble vitamin. For determinatiom was used coulometric detector Coulochem III. Analysis overshoot on column Lichrospher 60, RP - select B (240 x 4,0 mm and.d., 5 em), Merck. Mobile phase was composed of acetic acid : acetonitrile (CH3COOH 0,2410 mol/l; pH 3,0) 85: 15. Flow rate was 1ml/min, in temperature 30žC. Current inserted on working electrode was 900 mV, sensitiveness 200mV.
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Analytical evaluation of the pharmaceutical formulations using chromatographic methods II
Sinkoviczová, Magdalena ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
Analytical drug evaluation by chromatographical methods II. ( Determination of ambroxol in pharmaceutical preparation ) Diploma paper Magdalena Sinkoviczová Charles University in Prague, Pharmaceutical Faculty in Hradec Králové, Department of pharmaceutical chemistry and drug control In this diploma paper is described elaboration of one possible method of HPLC analysis of ambroxol and methylparaben ( and its degradation product, p- hydroxybenzoic acid ) in pharmaceutical preparations. Optimal results are provided by analysis made on column Separon SGX C 18 from Tessek, using mobile phase in composition acetonitril : phosphate buffer ( KH2PO4 0,08 mol/l; pH 5,8 ) 40:60 v/v, with flow rate of 0,5 ml/min. Detection was performed at 254 nm by UV detector. For verification of linearity was used a method of calibration curve, constructed from results from analysis of five solutions with various concentration of components. Precision was verified by analysis of six solutions simulating real composition of pharmaceutical preparation. Validation was performed using propylparaben as internal standard. This metod was used for quantification of MUCOSIN® components. Amount of ambroxol was determined on 7,5642 mg/ml which corresponds to 100,86 % of declaration amount ( 7,5 mg/ml ). The amount of methylparaben...
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Analytical evaluation of the pharmaceutical formulations using chromatographic methods I
Hladík, Michal ; Mokrý, Milan (advisor) ; Kastner, Petr (referee)
Analytical evaluation of the drugs using chromatographic methods I. (Determination of the conditions for simultaneous evaluation of clotrimazole and benzylalcohol) Thesis Michal Hladík Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Analysis Optimum chromatographic conditions for simultaneous HPLC determination of clotrimazole and benzylacohol in a pharmaceutical formulations (2 % cream) were elaborated. The best results was achieved using chromatographic column Separon SGX CN, 7 μm, 150 x 4 mm I. D. (Tessek Prague, Czech Republic). The mobile phase consisted of mixture of acetonitrile and aqueous solution of K2HPO4 0.05 mol/l (60 : 40), pH 6.7 (adjusted with 10 % H3PO4). The flow rate was 0.8 ml/min. The UV detector set at 268 nm was used. Method was validated for linearity and robustness. Complete validation will be an aim of the next rigorous work.
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HPLC evaluation of compounds relative to clotrimazol
Topková, Kateřina ; Mokrý, Milan (referee) ; Kastner, Petr (advisor)
HPLC Determination of Related Substances of Clotrimazole Academic dissertation Mgr. Kateřina Topková Charles University in Prague, Faculty of Pharmacy in Hradci Králové, Department of Pharmaceutical Chemistry and Drug Control A suitable method for determination of impurities (imidazole, (2-chlorphenyl)diphenylmethanol, unknown impurities) content in vaginal cream using High Performance Liquid Chromatography was searched. The best results were obtained with chromatography column DISCOVERY® HS F5, 5 μm, 4,5 × 150 mm together with the pre-column DISCOVERY® HS C18, 5 μm, 2,1 × 20 mm, mobile phase acetonitril: buffer (K2HPO4 0,05mol/l, pH = 6,1 set up by 85% H3PO4) 60:40. Flow rate was 1,0 ml/min. UV detector for the determination with the setting wave length 223 nm was used. The total time of the analysis was shorter than 10 minutes. Substances were eluated in the following order: imidazole, clotrimazole and (2-chlorphenyl)diphenylmethanol.
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HPLC evaluation of selected drugs I
Skryjová, Denisa ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
61 ABSTRACT HPLC evaluation of selected drugs I. THESIS Denisa Skryjová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this thesis were developed the optimum chromatographic conditions for simultaneous HPLC analysis of tramadol and paracetamol in combined tablet. The chromatographic column Discovery HS F5, 5 µm, 150×3 mm I.D. made by Supelco was chosen as the stationary phase. Mobile phase mixture formed acetonitrile : ammonium acetate solution 0.005 mol/l, acidified with acetic acid at pH 3.2 in the ratio 20:80 (v/v), at a flow rate of 1.0 ml/min. Acetylsalicylic acid was used as an internal standard. Detection took place at λ = 270 nm using a UV detector. The compounds were eluted in order of paracetamol, acetylsalicylic acid and tramadol.
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Analytical evaluation of drugs using chromatographic methods VI.
Boudová, Kristýna ; Mokrý, Milan (advisor) ; Kastner, Petr (referee)
Analytical evaluation of drugs using chromatographic methods VI. Diploma thesis Kristýna Boudová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of pharmaceutical chemistry and drug analysis. There was worked out the method for simultanious determination of vitamins B1 (thiamine), B3 (nicotinamide), B6 (pyridoxine) a vitamin C (ascorbic acid) using high performance liquid chromatoghaphy in multivitamin tablets in this work. This method was used for determination of these vitamins in effervescent multivitamine substance used as food supplement. Acquired results were compared with value declared by the producer. Best results were reached by using chromatographic column Lichrosphere 100 RP C18, 250 mm x 4 mm I.D. (5 µm) Merck, Germany with mobile phase methanol : water (pH adjusted to 2,8 by acetic acid 10%) 0,005 mol/l sodium hexanesulfonic acid + 0,1% triethylamine) in proportion 20:80 (v/v). There was used spectrofotometric detector with wavelenght 270 nm for detection. Flow rate was 1 ml/min, time of analysis didn't exceed 13 minutes. Substances were eluated in order: ascorbic acid, nicotinamide, pyridoxine and thiamine. The method will be validated.
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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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HPLC analysis of drugs and drug candidates in biological material
Luňáková, Veronika ; Kovaříková, Petra (advisor) ; Mokrý, Milan (referee)
High-performance liquid chromatography (HPLC) is currently one of the most progressive separation methods, permitting, simultaneously, both quantitative and qualitative analysis. An important area for the utilisation of HPLC is the identification of drugs and their metabolites in biological materials. This study was focused on the development of chromatographic conditions appropriate for HPLC analysis of two new potential drugs derived from aroyl-hydrazone, HNAF-INH and 4,6DAR-INH, in biological material and its subsequent application in the assessment of the stability of these substances in plasma. Analysed chelators were prepared by the modification of the structure of salicylaldehyde isonicotinoyl hydrazone (SIH) with the purpose of improving the stability of the substance in plasma. As a suitable stationary phase the HPLC column LiChroCART® HPLC - cartridge LiChrospher®100 RP - 18e (15μm) with the pre-column LiChroCART® 4-4 Purospher® RP - 18 (5μm) was chosen. The mobile phase in this case represented by a HNAF-INH compound: phosphate buffer (0,01 mol/l aqueous solution of NaH2PO4 · 2 H2O with 2 mmol/l EDTA, pH 3) : methanol, 42:58 (v/v). The temperature in the column was 25řC, the flow rate 1,0 ml/min and UV detection was performed at 288 nm; SIH was used as an internal standard. The mobile...
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