Abstract
The aim of this study was to establish an improved isocratic RP-LC-DAD method for separation and determination of rizatriptan benzoate and its two degradation products, L-749.019 and L-783.540 in tablets. Since the chromatographic behavior of target substances can be influenced by various experimental parameters, the whole study was carried out by employing experimental design methodology. The investigation included the influence of mutual changes of the mobile phase composition (methanol amount in the range 3–7% and pH of the water phase from 5.0 to 6.0) and the temperature (from 20 to 30 °C). The response surface design by means of Box-Brehnken design was used to obtain a predictive model which describes the changes in the response within the experimental domain. Additionally, several different target responses were evaluated and Derringer’s desirability function was used for reaching a suitable compromise among the responses. This multi-criteria decision making approach is based on constructing a desirability function for each individual response and afterwards establishing the overall desirability function. Such methodology provided us with the best operating conditions, satisfactory resolutions between the analytes and the shortest possible total analysis time. The experiments were performed on C18 XTerra (150 mm × 3.9 mm), 5 μm column with the mobile phase consisting of a mixture of methanol, TEA and 0.01 mol L−1 KH2PO4 (6:9.4:84.6 v/v) pumped at a flow rate of 1.2 mL min−1, pH of the water phase adjusted to 6 with 85% orthophosphoric acid, a column temperature of 20 °C and detection at 225 nm. Afterwards, the new method was validated and subsequently applied in analysis of commercially available rizatriptan tablets.
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This research was supported by the Ministry of Science and Environmental Protection of the Republic of Serbia as the part of the project “Synthesis, Quantitative Structure/Properties and Activity Relationship, Physical-Chemical Characterization and Analysis of Pharmacologically Active Substances” No. 142071 B.
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Zečević, M., Jocić, B., Živanović, L. et al. Application of Multicriteria Methodology in the Development of Improved RP-LC-DAD for Determination of Rizatriptan and Its Degradation Products. Chroma 68, 911–918 (2008). https://doi.org/10.1365/s10337-008-0823-z
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DOI: https://doi.org/10.1365/s10337-008-0823-z