Comparative study of different approaches to the determination of robustness for a sensitive-stacking capillary electrophoresis method. Estimation of system suitability test limits from the robustness test

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• 作者：Teresa Galeano-Díaz ; María-Isabel Acedo-Valenzuela ; Nielene Mora-Díez and Antonio Silva-Rodríguez
• 关键词：Robustness test ; Sensitive ; stacking capillary electrophoresis method ; Plackett–Burman design ; System suitability test limits
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2007
• 出版时间：September, 2007
• 年：2007
• 卷：389
• 期：2
• 页码：541-553
• 全文大小：257 KB
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Food Science
  Inorganic Chemistry
  Physical Chemistry
  Monitoring, Environmental Analysis and Environmental Ecotoxicology
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1618-2650

文摘

A robustness study for a sensitive-stacking capillary electrophoresis method based on “acetonitrile-stacking” was carried out. Ten variables (pH, acetonitrile and triethanolamine in the buffer, injection time, injection pressure, acetonitrile and NaCl in the sample, capillary and tray temperature and separation voltage), whose levels were varied by 10% around the nominal level, were examined by a Plackett–Burman design (two-level design). The effects on corrected peak area and resolution (responses) were calculated and interpreted using three statistical approaches: dummy variables, distribution effects (Dong’s algorithm) and calibration curve. Dong’s method was found to be the most suitable to evaluate the robustness, since it considers qualitative (resolution) and quantitative (corrected peak area) responses and does not need a minimum number of dummy variables in the experimental design. From these studies, we can deduce that the first four variables were significant at 10% around the nominal level, and therefore a new design was made with those four variables at 5% nominal level. Then, only two variables proved to be significant for the resolution between some peaks, so the system suitability test limits were defined for these resolutions.