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Validation of chromatographic methods in pharmaceutical analysis
Kegkeroglou, Iokasti ; Kučera, Radim (advisor) ; Kastner, Petr (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Pharmaceutical Analysis Student: Iokasti Kegkeroglou Supervisor: doc. PharmDr. Radim Kučera, Ph.D. Title of Thesis: Validation of chromatographic methods in pharmaceutical analysis Validation is an integral part of every analytical method. Its aim is to demonstrate that the method is suitable for the intended use. This work provides an overview and comparison of documents related to the validation of bioanalytical methods. The work includes guidelines that are currently valid in Europe, the USA or have general validity. At first, attention is paid to the history and developments in this area. Subsequently, the parameters that need to be tested in the validation study are described and are divided according to the regulatory authorities. The following chapter compares the latest versions of the guidelines regarding the validation of separation bioanalytical methods issued by the EMA, FDA, and ICH. Although the individual methodologies are similar in many aspects, there are still differences among them. Hopefully, the differences will be eliminated in the framework of harmonization and only one methodological guideline could be used worldwide. Finally, it follows a detailed statistical evaluation of...
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Electrophoretic determination of rivaroxaban
Petrák, Ondřej ; Křížek, Tomáš (advisor) ; Kubíčková, Anna (referee)
Capillary electrophoresis is a method used in pharmaceutical analysis because of its low cost, speed and environmental friendliness. This diploma thesis deals with development of electrophoretic method for rivaroxaban determination. After several optimizations, a method suitable for rivaroxaban determination inside its dosage forms was developed. Optimizations involved change of background electrolyte's composition from aqueous solution of low molecular weight organic acids to non-aqueous solution of acetic acid and cetyltrimethylammoniumbromide in acetonitrile in multiple steps. Final conditions of analysis included background electrolyte composed of 1M acetic acid and 40mM cetyltrimethylammoniumbromide in acetonitrile, sample injection carried out hydrodynamically by pressure of 5,0 kPa for period of 3 s and subsequent insertion of separation voltage of 30,0 kV for entire duration of analysis. Capillary content was mobilized by pressure of 0,50 kPa for entire duration of analysis. With aforementioned optimizations a selective method for determination of dosage forms of rivaroxaban was obtained. This method provides limit of detection 0,0056 mg/ml and limit of quantification 0,019 mg/ml and is linear in 0,01 - 0,40 mg/ml range with a recovery of 93,2 %. Keywords capillary electrophoresis,...
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