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Evaluation of biologically active substances using HPLC V.
Kokošková, Denisa ; Pilařová, Pavla (advisor) ; Mokrý, Milan (referee)
Determination of the Biologically Active Substances using High Liquid Chromatography V. Thesis Denisa Kokoškova Charles University in Praque, Faculty of Pharmacy in Hradci Králové Department of Pharmaceutical Chemistry and Drug Control In this thesis was optimized determination method of salicylic acid, as the main decomposition product, from acetylsalicylic acid, which is presented in Acylpyrin, Acylcoffin and Acifein. For evaluation was used high performance liquid chromatography with electrochemical detection. Through monolithic column was analyzed Phenomenex 100 x 4,6 mm, Onyx monolithic C8. Optimization and verifying of suggested conditions electrochemical detection was focused on exploration of mobile phase and sample dissolvent. Suitable mobile phase was 50mM phosphate buffer liquid (pH 2,5) and acetonitrile in ration 80 : 20. Flowing throw column was 1ml/min, temperature 25řC, injected volume 10 μl. Electrical potential was adjusted to values E1= 300 mV, E2= 850 mV. Range was 1 μA. Optimized method was validated, parameters were precision, accuracy, linearity, specificity, robustness, limit of quantitation and limit of detection. The sample stability of Acylpyrin tablets was monitored for 48 hours.
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HPLC EVALUATION OG FUMAGILLIN IN THE MEDICINE
Strýčková, Kristýna ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
HPLC EVALUATION OG FUMAGILLIN IN THE MEDICINE Rigorous thesis Mgr. Kristýna Strýčková Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this rigorous thesis is described analytic evaluation of fumagillin by using HPCL and stated the amount of fumagillin in the medicine. The measurment was implemented on chromatographic colony in size 3 x 150 mm I.D. with the Seladon SGX NH2 filling, 7μm. There was used the mobile phase composed of methanol: amonium acteate (aqueous solution 0,005 mol/l, v/v )in the ratio of 60:40, at the flow rate of 1ml/min and pressure of 2,5-2,6 MPa. The detection was performed at 335 nm using the UV detektor. The samples were spraeyd in cubage 20 μ/l. The international standard method was drawn up for determination of fumagillin in medicine. The most suitable sample from the selected conditions was nimesulid. Concerning validation parameters were verified linearity, accuracy, robustness, selection and detector limit. Further there was examined the stability in conditions of room temperature and the temperature od 2-8˚C. It was determined 0,0238 g of fumagillin in 1 g of medicine that is stated as 95,2% of neccessary amount.
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Study on possible utilization of metal oxide based stationary phases for the analysis of polar compounds
Slaninová, Jitka ; Kovaříková, Petra (advisor) ; Mokrý, Milan (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Student: Jitka Slaninová Supervisor: Doc. PharmDr. Petra Kovaříková, Ph.D. Title of diploma thesis: Study on possible utilization of metal oxide based stationary phases for the analysis of polar compounds This diploma thesis is aimed at investigation of the ability of zirconia (column ZirChrom®-PHASE, 150 x 4,6 mm; 5 µm) and titania (column Sachtopore®-NP, 150 x 4,6 mm; 5 µm) based stationary phases for analyses under the conditions of hydrophilic interaction chromatography (HILIC). Influence of mobile phase strength, mobile phase pH and buffer strength on the separation of biologically important polar compounds: adenosine monophosphate (AMP), adenosine diphosphate (ADP), adenosine triphosphate (ATP), cyclic adenosine monophosphate (cAMP), creatine (C) and phosphocreatine (CP) was tested. All analyses were performed using isocratic elution. The mobile phases consisted of an organic part - acetonitrile (ACN) and an aqueous part - buffer (sodium phosphate dibasic - Na2HPO4 with sodium fluoride - NaF) in different ratios. The mobile phase flow rate was at 1 mL/min. The detection of analytes was performed by using a photodiode array detector at wavelengths of 215 nm for C and CP...
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Determination of Selected Active Substance in the Preparation VII.
Šalamounová, Anna ; Kastner, Petr (advisor) ; Mokrý, Milan (referee)
Determination of Selected Active Substance in the Preparation VII Thesis Anna Šalamounová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control Suitable HPLC methods for the determination of cinchocaine and for the determination of purity of dexamethasone in liquid pharmaceutical preparation were searched. The monolithic column Chromolith Speed ROD RP-18e 50-4.6 was used. A mixture of water:acetonitrile; 50:50; 1,575 ml of triethylamine in 250 ml of water; was chosen as the mobile phase for cinchocaine hydrochloride; pH of the mobile phase was adjusted to 7.0 by orthophosphoric acid. Flow rate was 3 ml/min, column temperature 25 žC, injected volume 5 µl and UV detection at 325 nm. Linearity, specificity, precision and accuracy were tested under these conditions. For purity of dexamethasone gradient elution was chosen. Mobile phase A: water, acetonitrile (80:20) and mobile phase B in the rate of 93:7; pH of the mobile phase was adjusted to 7.0 by orthophosphoric acid. Mobile phase B: water, acetonitrile (75:25); 1,05 ml triethylamine in 250 ml water; pH of the mobile phase was adjusted to 7.0 by orthophosphoric acid. Flow rate was 4 ml/min, column temperature 25 žC, injected volume 50 µl and UV detection at 238 nm. The method was...
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Determination of Camphor Content in the Ointment Using Monolithic Column
Voříšková, Michaela ; Kastner, Petr (advisor) ; Mokrý, Milan (referee)
Determination of Camphor content in the ointment using monolithic column Thesis Mgr. Michaela Voříšková Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control The HPLC method for determination of camphor content in pharmaceutical preparation Unguentum camphoratum vaselinatum 10% using monolithic column was developed. The time of analysis was shorted on 1,3 min. The chromatographic column Chromolith Speed rod, RP-18e 50-4,6 mm and chromatographic precolumn Chromolith, RP-18e 10-4,6 mm with mobile phase water : methanol 35 : 65 were used. UV detector for the determination with the setting wave lenght 289 nm was used. The metod was validated for accuracy (recovery = 99,03 %), precision (RSD = 0,83 %), linearity (R = 0,9995) and for specificity. The metod was also tested in other pharmaceutical preparations containing camphor.
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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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Employment of HPLC in the field of drug analysis II.
Holásková, Petra ; Kučera, Radim (advisor) ; Mokrý, Milan (referee)
VYUŽITÍ HPLC V ANALÝZE LÉČIV II. PETRA HOLÁSKOVÁ 69 Vitamins are natural substances found in plants and animals. With few exceptions, the human body cannot synthesize them. Consequently, they must be supplied by the diet or by dietary supplements. Vitamins are essential for the normal growth, vitality, and for the prevention and cure of many health problems and diseases together with other essential nutrients such as proteins, fatty acids and carbohydrates. Vitamins are required only in tiny amounts by organism (micrograms or milligrams per day). Therefore, the methods for their separation and determination should be very sensitive. One possible method is the high performance liquid chromatography equipped with the electrochemical detection. This Diploma Thesis is focused on finding of optimal conditions for separation of folic acid, biotin and vitamin B12. These water-soluble substances belong to the B group vitamins. Their main sources are meat, eggs, brewer's yeast or pulses. The separation was carried out on chromatography column Lichrospher 60, RP - select B (240 x 4.0 mm i.d., 5 μm) obtained from Merck. The analysis was achieved by using the electrochemical detector Coulochem III with sensitivity of 1 μA. The flow rate was set to 1 ml/min and the current inserted on the working electrodes was 600 mV...
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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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The different extraction techniques using for HPLC evaluation of some drugs
Kračmarová, Alžběta ; Mokrý, Milan (advisor) ; Pohanka, Miroslav (referee)
In this study the reversed-phased HPLC method for determination of an atypical antipsychotic drug amisulpride in a rabbit plasma was developed. The amisulpride is a benzamide derivative, which antagonizes human dopamine D2/D3 receptors. The main clinical efficacy of this drug is the therapy of both negative and positive symptoms of schizophrenia and low propensity to produce extrapyramidal sight effects. A Separon SGX C18 (size of particles 7 μm) as a stationary phase, a mixture of an acetonitrile - 0,1M amonium acetate (pH 5,6) 40:60 (v/v) as a mobile phase and an ambroxol as an internal standard were used for the analysis. Before the determination a solid-phase extraction was made. The method is linear in concentrations between 200 and 800 ng/ml (y=0,0065x-0,0695, r2 =0,9930), selective and robust. The analysis time was 11 min. A teoretical part of this study is approached to methods of an extraction, which is a very important step in an analysis of a biological material.
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