Abstract
Topicality. Robustness tests were originally introduced to avoid problems in interlaboratory studies and to identify the potentially responsible factors. The aim of this study was the rubustness evaluation of the chromatographic determination of nifedipine in medicines using Youden’s test.Materials and methods. Youden’s test is a reliable method to evaluate the robustness of analytical methods, by means of an experiment design which involves seven analytical parameters combined in eight tests. In the present study, we assessed the robustness of a chromatographic method to quantify nifedipine using Youden’s test. Youden’s test showed to be a simple and feasible procedure to evaluate the robustness of chromatographic methods.Results and discussion. Using the criteria of Youden’s test, the chromatographic method showed to be highly robust regarding of nifedipine content, when variations in seven analytical parameters were introduced. The highest variation in nifedipine content was 0.28 %, when the concentration of trifluoroacetic acid in the mobile phase was altered; a value considerably low and not significant in routine analyses. Conclusions. Youden’s test showed to be a reliable and useful tool for the robustness evaluation of the chromatographic method for assay of nifedipine. Therefore, Youden’s test can be successfully applied for the robustness evaluation in validation process of analytical methods by HPLC.
Highlights
Both the ICH and the USP guidelines define the robustness of an analytical procedure as a measure of its capacity to remain unaffected by small but deliberate variations in procedural parameters listed in the documentation, providing an indication of the method’s or procedure’s suitability and reliability during normal use
Youden’s test is a reliable method to evaluate the robustness of analytical methods, by means of an experiment design which involves seven analytical parameters combined in eight tests
Using the criteria of Youden’s test, the chromatographic method showed to be highly robust regarding of nifedipine content, when variations in seven analytical parameters were introduced
Summary
Both the ICH and the USP guidelines define the robustness of an analytical procedure as a measure of its capacity to remain unaffected by small but deliberate variations in procedural parameters listed in the documentation, providing an indication of the method’s or procedure’s suitability and reliability during normal use. Robustness tests were originally introduced to avoid problems in interlaboratory studies and to identify the potentially responsible factors. This means that a robustness test was performed at a late stage in the method validation since interlaboratory studies are performed in the final stage. Performing a robustness test late in the validation procedure involves the risk that when a method is found not to be robust, it should be redeveloped and optimised. Other wider alternative to determine the robustness of analytical methods is the Youden’s test This test allows evaluating the method robustness and pointing out the influence of each analytical parameter in the final results. The basic idea of Youden’s test is not to study one alteration at time but to introduce several changes at once, in such a manner that the effects of individual changes can be ascertained [2, 3]
Sign-in/Register to view highlights & summary Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
