| Abstract |
The aim of the present dissertation is the development and the validation of a method for the analysis of the formulation SPLENTIR. The drug SPLENTIR is an analgesic-painkiller which is widely used in the pharmaceutical market. Despite its widespread use, there is no published validated analytical method capable to provide quantitative information on the composition of the commercial formulation. Initially the development of the analytical protocol is described, and which is based on reversed phase chromatography (HPLC). Subsequently the analytical data is statistically analyzed for the completion of the method validation.
The developed methodology is based on the optimization of three basic sets of parameters. The first one deals with the rational choice of the mobile phase for optimum chromatographic separation. The second optimized parameter is the pH of the mobile phase. The third set includes the optimization of the physical parameters and includes the pressure the temperature and the flow rate of the mobile phase. Finally the wavelength of the detector is optimized in order to obtain the best detection sensitivity for all three analytes.
The implementation of the optimized experimental conditions provides a highly consistent and accurate chromatographic method for the analysis of the pharmaceutical formulation. The use of this method is of paramount importance for the facile, accurate and expedient drug screening for market release. The total time required for the completion of the analysis of the specific formulation requires just 7 minutes. The three major chromatography peaks observed were successfully assigned to the corresponding three active compounds of the SPLENTIR formulation. More specifically it was found that the retention times for acetylsalicylic acid, the paracetamol and the caffeine are 7.0, 3.5 and 4.0 minutes respectively under the specific experimental conditions used during the developed method.
The analytical parameters that are required for the validation of the method development are i) the linearity of the method, for which calibration curves of the active compounds are calculated, ii) the accuracy of the method, iii) the precision of the method, iv) the working range, and finally v) the detection limit. The method developed for the analysis of SPLENTIR in this work was successfully validated based on the excellent results obtained from the statistical analysis of the chromatographic data for all the validation parameters required.
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Ανάπτυξη και διαπίστευση μεθόδου ανάλυσης του splentir με RP-HPLC
