|
|
Valuation of the biologically active substances by liquid chromatography IX.
Sommernitzová, Nora ; Pilařová, Pavla (advisor) ; Kastner, Petr (referee)
Valuation of the biologically active substances by high performance liquid chromatography II. (Validation of determination of metformin-hydrichloride by high performance liquid chromatography) Thesis Sommernitzová Nora Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control The method for determination of the metformin-hydrochloride by high performance liquid chromatography in pharmaceutical preparations Diaphage 500 and Diaphage 850 was optimalised. Using the principle of ion exchange chromatography, the metod was carried out on the μBondapack C18 (10μm) column. A mobile phase composed of sodium pentanesulfonate and sodium chloride at a flow rate 1,5 ml/min was used for the separation. pH was adjusted to 3,5 using phosphoric acid. The temperature was set at 25,0 řC. Detection was carried out at 218 nm. Following these conditions the metod was validated. The accuracy, precision, linearity and specifity were also verified. All tested parameters satisfied the criterions.
|
|
|
Evaluation of biologically active substances using liquid chromatography XV
Blažková, Zuzana ; Pilařová, Pavla (advisor) ; Kastner, Petr (referee)
Charles University in Praque, Faculty of Pharmacy in Hradci Králové Department: Pharmaceutical Chemistry and Drug Control Candidate: Zuzana Blažková Tutor: Mgr. Pavla Pilařová Ph.D. Name of Degree Paper: Evaluation of biologically active substances by High- Performance Liquid Chromatography XV. The new, quick and sensitive method for assessment of risperidone and its related substances in pills was developed. The ultra-effective liquid chromatography with UV/VIS detection in 260 nm was used. The analysis was proceeded in the colony of Syncronis C18 10x3 mm with the size of the particles 1,7 µm, in the temperature of 40 řC .The mobile stadium was created by acetonitrile and by acetate regulator and the gradient elution with the flow of 0,5 ml/min was used. The final method was used in stress loading that had the form of the hourly ebuliency with water. Key words: UHPLC,chromatography, risperidone
|
|
|
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...
|
|
|
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.
|
|
|
Analytical evaluation of active substances liquid chromatography VI.
Kuželová, Kristýna ; Pilařová, Pavla (advisor) ; Kastner, Petr (referee)
ANALYTICAL EVALUATION OF ACTIVE SUBSTANCES BY LIQUID CHROMATOGAPHY VI. Diploma Thesis Kristýna Kuželová Charles University in Prague, Faculty of Pharmacy in Hradec Kralove, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové The method for determination of the piroxicam in rabbit plasma using solid phase microextraction (SPME) and high performance liquid chromatography (HPLC) with UV detection was optimalized. Fiber coated with PDMS/DVB was used for microextraction. Isoxicam was chosen as an internal standard. The sample of plasma was adjusted to pH 2,5. Microextraction was composed of 20 minutes sorption and 20 minutes desorption into 200 μl of methanol. Column with reversed phase C18 was used for separation. A solution of water and acetonitrile (60:40 v/v) was used as the mobile phase. Its pH was adjusted to 2,5 using formic acid. The flow rate was 1 ml/min and temperature on the column was set at 40řC. The detection was carried out at 333 nm. Linearity and selectivity of the method were verified. Detection and quantification limits for piroxicam were also determined.
|
|
|
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...
|
|
|
Evaluation of Impurity in Pharmaceutical Preparation
Topková, Kateřina ; Kastner, Petr (advisor) ; Pilařová, Pavla (referee)
Evaluation of Impurity in Pharmaceutical Preparation (Determination of Imidazol Content with HPLC) Thesis 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 imidazol content and eventually simultaneous determination of benzylalcohol and imidazol contents in vaginal cream using High Performance Liquid Chromatography was searched. The best results were reached on chromatography column LiChrospher RP 18,5 μm, 125 mm x 4,6 mm with mobil phase methanol: buffer with Sodium hexansulphonate 30 : 70; pH 7 and flow 1,0 ml/min. UV detektor for the determination with the setting wave length 223 nm was used. The total time of the analysis was shorter than 20 minutes. Substances were eluated in the following order: imidazol, benzylalcohol, clotrimazol.
|
|
|
Evaluation of Stability of Gestodene Using HPLC
Oháňková, Alena ; Kastner, Petr (advisor) ; Pilařová, Pavla (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Pharmaceutical Analysis Candidate: Alena Oháňková Supervisor: PharmDr. Petr Kastner, Ph.D. Title of thesis: Evaluation of Stability of Gestodene Using HPLC The purpose of this thesis was to develop and validate the HPLC method and further evaluate the stability of gestodene under selected model conditions. Gestodene is highly effective new- generation gestagen that is a part of hormonal contraceptives that subsequently occurs in low concentrations in surface waters. The default parameters set in Czech pharmacopoeia were used for the further development of the suitable evaluation method. The chromatographic parameters were optimized in order to obtain the method that would reduce time and costs. The developed isocratic method has shortened the retention time of gestodene by half without interfering with the dead retention time of the column and has met all prescribed validation requirements. The chromatographic parameters of the developed method are as follows: column (length 150 mm, internal diameter 4.6 mm), stationary phase (octadecylsilylated R (5 μm) spherical silica gel, mobile phase (water R, acetonitrile R1), elution (isocratic, 45 % water + 55 % acetonitrile), flow rate (1 ml/min),...
|
|
|
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.
|
|
|
GC analysis of drugs with utilization of ionic liquid as a stationary phase I
Bärová, Karolína ; Kastner, Petr (advisor) ; Kučera, Radim (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Pharmaceutical Analysis Supervisor: PharmDr. Petr Kastner, Ph.D. Student: Karolína Bärová Title of Thesis: GC analysis of drugs with utilization of ionic liquid as a stationary phase I In this thesis, we focused on testing of three commercially obtainable columns with ionic liquids as stationary phases, which we tested on a model sample of ibuprofen and its four pharmacopoeial impurities after derivatization by alkylchloroformates. The results obtained on these columns were compared to results obtained on column with conventional nonpolar stationary phase. Furthermore, we tried to describe and explain retention mechanisms, which were important in these separations, we also tried to optimize methods for our individual columns and extract our derivatives into a nonpolar phase, with the view to diminishing the harmful effect of samples on columns. We appraise the results obtained on ionic liquid stationary phases and on a nonpolar stationary phase as quite comparable. The analysis of our derived samples can be performed on all tested ionic liquid columns and the analysis can be optimized for all of them. Apart from the change in selectivity on the most polar stationary phase, we did not notice any great...
|
guest ::
