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Using of core-shell columns for miconazole determination
Hloušková, Martina ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
BSc. Martina Hloušková Supervisor: Ing. Martin Drastík, Ph.D. The aim of this diploma thesis was the optimization and validation of a HPLC method for miconazole determination in samples supplied by the Department of Pharmaceutical Technology. A gradual miconazole release dependent on the composition of the copolymere of glycolic and lactic acid was studied. HPLC analysis was performed using a modern core-shell Column Ascentis Express RP- Amide, 10 cm x 3.0 mm; 2.7 μm. Optimized analytical conditions were: mobile phase methanol:water 70:30, flow rate 0.8 ml/min, temperature 45 řC, injection 5 l and UV detection at 220 nm. Miconazole retention time was 5.65 min. The entire analysis was carried out in 7 minutes. When the optimal conditions of analysis were determined, the method could be validated. The following parameters were monitored during validation: linearity, selectivity, efficiency, LOD, LOQ, repeatability and tailing factor. All of the monitored parameters met the requirements of the Czech Pharmacopoeia.
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Simplification of terbinafine HPLC analysis of samples based on biodegradable polyesters
Malovaná, Andrea ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Andrea Malovaná Supervisor: Ing. Martin Drastík, Ph. D. Diploma thesis: Simplification of terbinafine HPLC analysis of samples based on biodegradable polyesters A HPLC method for determination of terbinafine in samples consisting of copolymers of lactic and glycolic acid was optimized and validated. The development of the method was based on the finding of suitable chromatographic conditions for separation of terbinafine. The separation was performed on the Ascentis Express ES-CN, 15 cm × 4.6 mm; 2.7 μm core- shell column. The mixture of the citrate phosphate buffer pH 4 and acetonitrile in ratio 40:60 (v/v) was chosen as the mobile phase. The mobile phase flow rate was set to 1.4 ml/min and the temperature to 30 řC. The injection volume of samples containing terbinafine was 5 µl. The UV detection at 226 nm was employed. The retention time of terbinafine was 3.3 min. The whole analysis was completed within 4 min. The method was validated, following parameters were tested: column efficiency, factor of symmetry, LOD, LOQ, linearity, repeatability and robustness. Keywords: terbinafine, HPLC, core-shell column, PLGA
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Using of core-shell columns for fluconazole determination
Brokešová, Kateřina ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Kateřina Brokešová Supervisor: Ing. Martin Drastík, Ph. D. Thesis title: The use of core-shell columns for fluconazole determination A novel HPLC method for determination of fluconazole in dissolution test samples was developed and partly validated. A matrix formed by lactic and glycolic acid copolymer branched by different compounds was used as a drug carrier. Fluconazol was incorporated as the model drug. The concentration profile of fluconazole was studied by developed HPLC method during the dissolution test. A modern core-shell column Ascentis Express RP-Amide, 10 cm × 3.0 mm; 2.7 μm was employed. A mixture of acetate buffer pH 5.0:methanol (80:20) served as the mobile phase. The flow rate was 0.70 ml/min and the detection wavelength was 260 nm. The temperature of analysis was 50 řC. The retention time of fluconazole was 3.3 min and the whole analysis took just 4 min. Keywords: fluconazole, core-shell column, HPLC, PLGA
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Determination of steviol glycosides by HPLC
Hollá, Marcela ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Marcela Hollá Supervisor: Ing. Martin Drastík, Ph.D. Title of Diploma Thesis: Determination of steviol glycosides by HPLC A new HPLC method was developed and validated for simultaneous detemination of major steviol glycosides stevioside and rebaudioside A in food supplements. Separation took place in hydrophilic interaction chromatography mode on column with core-shell particles. The method was aplicated on analysis of steviol glycosides in products Valosun, SlaDIA, Solia and extract from dried stevia leaves. Isocratic separation was performed using Kinetex 2,6u HILIC 100A, (100 x 2,1 mm; 2,6 µm), Phenomenex analytical column with mobile phase consisted of acetonitrile/0,05 M ammonium formate adjusted with formic acid to pH=3 in ratio 90:10, with flow rate 0,7 ml/min, column temperature set at 30 řC, pressure 19,8 MPa, UV detection at 203 nm and injection volume 1 µl. We compared the results of the analyzes with content of stevioside glycosides declared by the manufacturer. The new developed method allows rapid analysis of food supplements and plant extract containig steviol glycosides. Key words: steviol glycosides, stevioside, rebaudioside A, Stevia rebaudiana Bertoni, high...
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Using of core-shell columns for miconazole determination
Hloušková, Martina ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
BSc. Martina Hloušková Supervisor: Ing. Martin Drastík, Ph.D. The aim of this diploma thesis was the optimization and validation of a HPLC method for miconazole determination in samples supplied by the Department of Pharmaceutical Technology. A gradual miconazole release dependent on the composition of the copolymere of glycolic and lactic acid was studied. HPLC analysis was performed using a modern core-shell Column Ascentis Express RP- Amide, 10 cm x 3.0 mm; 2.7 μm. Optimized analytical conditions were: mobile phase methanol:water 70:30, flow rate 0.8 ml/min, temperature 45 řC, injection 5 l and UV detection at 220 nm. Miconazole retention time was 5.65 min. The entire analysis was carried out in 7 minutes. When the optimal conditions of analysis were determined, the method could be validated. The following parameters were monitored during validation: linearity, selectivity, efficiency, LOD, LOQ, repeatability and tailing factor. All of the monitored parameters met the requirements of the Czech Pharmacopoeia.
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Simplification of terbinafine HPLC analysis of samples based on biodegradable polyesters
Malovaná, Andrea ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Andrea Malovaná Supervisor: Ing. Martin Drastík, Ph. D. Diploma thesis: Simplification of terbinafine HPLC analysis of samples based on biodegradable polyesters A HPLC method for determination of terbinafine in samples consisting of copolymers of lactic and glycolic acid was optimized and validated. The development of the method was based on the finding of suitable chromatographic conditions for separation of terbinafine. The separation was performed on the Ascentis Express ES-CN, 15 cm × 4.6 mm; 2.7 μm core- shell column. The mixture of the citrate phosphate buffer pH 4 and acetonitrile in ratio 40:60 (v/v) was chosen as the mobile phase. The mobile phase flow rate was set to 1.4 ml/min and the temperature to 30 řC. The injection volume of samples containing terbinafine was 5 µl. The UV detection at 226 nm was employed. The retention time of terbinafine was 3.3 min. The whole analysis was completed within 4 min. The method was validated, following parameters were tested: column efficiency, factor of symmetry, LOD, LOQ, linearity, repeatability and robustness. Keywords: terbinafine, HPLC, core-shell column, PLGA
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Using of core-shell columns for fluconazole determination
Brokešová, Kateřina ; Drastík, Martin (advisor) ; Kubíček, Vladimír (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Kateřina Brokešová Supervisor: Ing. Martin Drastík, Ph. D. Thesis title: The use of core-shell columns for fluconazole determination A novel HPLC method for determination of fluconazole in dissolution test samples was developed and partly validated. A matrix formed by lactic and glycolic acid copolymer branched by different compounds was used as a drug carrier. Fluconazol was incorporated as the model drug. The concentration profile of fluconazole was studied by developed HPLC method during the dissolution test. A modern core-shell column Ascentis Express RP-Amide, 10 cm × 3.0 mm; 2.7 μm was employed. A mixture of acetate buffer pH 5.0:methanol (80:20) served as the mobile phase. The flow rate was 0.70 ml/min and the detection wavelength was 260 nm. The temperature of analysis was 50 řC. The retention time of fluconazole was 3.3 min and the whole analysis took just 4 min. Keywords: fluconazole, core-shell column, HPLC, PLGA
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