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The comparison of different types of stationary phases in HPLC analysis of medicament Diclofenac emulgel
Poláčková, Jitka ; Karlíček, Rolf (referee) ; Matysová, Ludmila (advisor)
The aim of this rigorous work is a comparison of different types of stationary phases for the analysis of the drug Diclofenac emulgel. It is necessary to take into account the many specialized materials from the pharmacopoeias, ICH guidelines and professional scientific journals in solution of the development of HPLC methodology, validation and choice of stationary phase analytical columns. Several types of stationary phases were tested, with the testing of conditions of the separation of active substances from the pharmaceutical formulation - diclofenac emulgel. The best results were placed on Discovery HS-F5 (15 cm x 4.6 mm, 5 m), time analysis was less than 4 minutes; Zorbax SB - CN (4.6 x 150 mm, 5 m) time of analysis was less than 5 min; Chromolith Performance RP - 18e (100 - 3 mm) time analysis was less than 3 minutes.
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Application of modern technologies for treatment of biological samples for HPLC analysis.
Dědečková, Klára ; Karlíček, Rolf (referee) ; Solich, Petr (advisor)
This diploma thesis is dealing with a using of new technologies for the treatment of biological material in the HPLC analysis. The main aim of this thesis was miniaturization of solid phase extraction process of blood serum on classical SPE columns to SPE plates for determination of liposoluble vitamins A and E by high performance liquid chromatography. The new extraction method for vitamin A and E in blood serum using the modern format of SPE plate was developed and optimized. This new method mineralizes a blood serum volume, makes sample treatment easy and can speed up the analysis.
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Development and Validation of Novel HPLC Methods for the Determination of Specific Analytes in Biological Material.
Urbánek, Lubor ; Solich, Petr (advisor) ; Karlíček, Rolf (referee) ; Nobilis, Milan (referee)
1. SUMMARY The presented dissertation thesis shows an interesting connection of two research fields that seem totally different from the first sight: analytical chemistry and medicine. However, the second sight could show that both branches might exist very closely to each other and their cooperation can be even useful for both sides. The initial part of the thesis deals with theoretical basics of HPLC and chromatographic instrumentation bringing a short overview of important principles of liquid chromatography including a brief introduction of crucial parts of an HPLC instrument. Due to the fact that the heart of the chromatographic system is an analytical column, another part of the text deals with different types of stationary phases and analytical sorbents. A separate chapter is focused on monolithic columns and other materials representing a new and original trend of chromatographic techniques. The main advantages and disadvantages of monolithic columns are then summarized in the published papers listed in the Experimental part (Enclosures 1, 2 and 9). Finally, the technical section of my thesis is concluded by a review of new trends in the chromatographic instrumentation presented e.g. by Ultra Performance Liquid Chromatography, columns filled with sub-2-micron particles or automatization or...
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Development and validation of HPLC methods for analysis of pharmaceutical formulations
Matysová, Ludmila ; Solich, Petr (advisor) ; Karlíček, Rolf (referee) ; Nobilis, Milan (referee)
7. Summary Development and validation of HPLC methods The doctoral thesis concerns with development of HPLC methods for analysis of pharmaceutical formulations, which meet all requirements for suitability, precision and reliability. Documentation of these parameters is called validation. At first theoretical principles of chromatography are described in this work, with the emphasis to liquid chromatography, included HPLC. The instrumentation in HPLC is described, mentioning the new trends in stationary phase's development - for example monolithic columns, zirkonia stationary phase, HILIC and sub-2-microns phases. In the other part UPLC system, one of the new trends in liquid chromatography development is discussed. Next part deals with the development of HPLC methods for analysis of pharmaceutics and is followed by chapter, in which analysis of pharmaceutical formulations is described, included preparation of the samples before analysis, stability monitoring and further the analysis of impurities. The last, relatively large chapter is dealing with the validation of analytical methods. Several institutions are concerned with validation requirements. They issue recommendation and/or guidelines, which are cogent for this process. In the Czech Republic there exists State Institute for Drug Control (SUKL -...
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Application of Sequential injection analysis in pharmaceutical analysis
Klimundová, Jana ; Solich, Petr (advisor) ; Blešová, Marie (referee) ; Karlíček, Rolf (referee)
SSUUMMMMAARRYY IINN EENNGGLLIISSHH This work is concerned on sequential injection analysis and its use in the field of pharmaceutical analysis. This flow method is a versatile, multi-purpose analytical system and for this is gaining more popularity in analytical chemistry. Firstly the review based on pharmaceutical applications was published. The new enhanced techniques such lab-on-valve, micro-SIA, bead injection and sequential injection chromatography was discussed. The experimental part is focused on the use of SIA for automation of long- lasting processes monitoring in pharmaceutical methods of analysis. Fully automated system for in vitro release testing of semisolid dosage forms was established. This test was based on Franz diffusion cell and its connection with SIA system. The system was tested for monitoring release profiles of three commercial preparations containing salicylic acid (Belosalic, Diprosalic, Triamcinolon S). The release profiles were statistically compared. The native fluorescence of salicylic acid was used for fluorimetric detection. Phosphate buffer pH 7.4 was the receptor medium, different membranes were tested. Samples were taken at 10 min intervals during 6 hours of the release test and each test was followed by calibration with five standard solutions. Other work was based on...
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