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HPLC separation of p-aminophenol, paracetamol, caffeine and propyphenazone on polar stacionary phase.
Maroušková, Alena ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
This thesis deals with finding optimal chromatographic conditions for a separation of p- aminophenol, paracetamol, caffeine and propyphenazon by HPLC. These analytes have different polarity and acidobazic properties. The application of traditional octadecylsilane stationary phases for their simultaneous determination is problematical. The PEG column have proved to be suitable for an efficient separation of the analytes with different polarities, i.e. with different chromatographic behavior. The resulting method brings shortening of analysis time, which is important for analysis of big series . Within the optimization of chromatographic conditions: a wide range of mobile phases has been tested (various organic solvents, various ratio of organic components to water phase components) a various level of acidity of the mobile phase has been tested ranging from 4 to 7 pH units various buffers have been tested behavior of the analytes has been tested under an enhanced temperature two PEG columns with different lengths have been tested Optimal chromatographic conditions for a separation of the analytes mentioned above, as well as the fulfillment of requirements for simplicity, analysis time and high degree of reliability have been found. The final chromatographic conditions: Stationary phase:...
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HPLC Method Development and Validation for Determination of Active Substances and Impurity in Valetol Preparation
Maroušková, Alena ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
This work extends the graduation thesis which found optimal chromatographic conditions for a separation of paracetamol, caffeine and propyphenazon, and the impurity p-aminophenol in the pharmaceutical preparation Valetol by HPLC method. At first, the benzoic acid was found as a suitable internal standard for the quantification. Next, the analytical method validation was carried out, including the suitability test of the chromatographic system. Within the suitability test of the chromatographic system the following attributes were tested: column efficiency expressed as a number of theoretic plates N assymetry of chromatographic peaks expressed as factor T resolution of chromatographic peaks reproducibility expressed as a relative standard error Within the analytic method validation were tested: precision linearity accuracy selectivity robustness stability The robustness test confirmed the analysis sensitivity to the change in the character of the mobil phase. As a part of the robustness test two parameters of mobile phase were tested: pH and triethylamine concentration changes. It was confirmed that the change of pH of the mobile phase influences mostly the retention times of p-aminophenol and benzoic acid. The change of triethylamine amount in the mobile phase influences mostly...
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HPLC Method Development and Validation for Determination of Active Substances and Impurity in Valetol Preparation
Maroušková, Alena ; Sklenářová, Hana (referee) ; Šatínský, Dalibor (advisor)
This work extends the graduation thesis which found optimal chromatographic conditions for a separation of paracetamol, caffeine and propyphenazon, and the impurity p-aminophenol in the pharmaceutical preparation Valetol by HPLC method. At first, the benzoic acid was found as a suitable internal standard for the quantification. Next, the analytical method validation was carried out, including the suitability test of the chromatographic system. Within the suitability test of the chromatographic system the following attributes were tested: column efficiency expressed as a number of theoretic plates N assymetry of chromatographic peaks expressed as factor T resolution of chromatographic peaks reproducibility expressed as a relative standard error Within the analytic method validation were tested: precision linearity accuracy selectivity robustness stability The robustness test confirmed the analysis sensitivity to the change in the character of the mobil phase. As a part of the robustness test two parameters of mobile phase were tested: pH and triethylamine concentration changes. It was confirmed that the change of pH of the mobile phase influences mostly the retention times of p-aminophenol and benzoic acid. The change of triethylamine amount in the mobile phase influences mostly...
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HPLC separation of p-aminophenol, paracetamol, caffeine and propyphenazone on polar stacionary phase.
Maroušková, Alena ; Sklenářová, Hana (referee) ; Šatínský, Dalibor (advisor)
This thesis deals with finding optimal chromatographic conditions for a separation of p- aminophenol, paracetamol, caffeine and propyphenazon by HPLC. These analytes have different polarity and acidobazic properties. The application of traditional octadecylsilane stationary phases for their simultaneous determination is problematical. The PEG column have proved to be suitable for an efficient separation of the analytes with different polarities, i.e. with different chromatographic behavior. The resulting method brings shortening of analysis time, which is important for analysis of big series . Within the optimization of chromatographic conditions: a wide range of mobile phases has been tested (various organic solvents, various ratio of organic components to water phase components) a various level of acidity of the mobile phase has been tested ranging from 4 to 7 pH units various buffers have been tested behavior of the analytes has been tested under an enhanced temperature two PEG columns with different lengths have been tested Optimal chromatographic conditions for a separation of the analytes mentioned above, as well as the fulfillment of requirements for simplicity, analysis time and high degree of reliability have been found. The final chromatographic conditions: Stationary phase:...
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