Assessment of liquid chromatographic method robustness by use of Plackett-Burman design

• Autorzy: Mašković M , Jančić-Stojanović B , Malenović A. , Ivanović D. , Medenica M.
• Języki publikacji: EN

Abstrakty

EN

Robustness testing is an important part of method validation. Many ideas on robustness testing can be found in the literature, but the most useful approach is application of experimental design. In the work discussed in this paper, Plackett-Burman design was used for robustness testing of an LC method. Robustness was assessed for a previously validated method developed for chromatographic analysis of perindopril tert -butylamine and its impurities. Eleven factors (seven real and four dummies) in twelve experiments were examined. Robustness was assessed by graphical (half-normal probability plots and Pareto charts) and statistical ( t -test) methods. For estimation of the standard error of effect (necessary for t -test estimation) calculations based on negligible effects and Dong’s algorithm were used at the significance levels α = 0.05 and α = 0.01. In this way the effect of the factors was completely defined and, furthermore, nonsignificant intervals for significant variables were calculated. Finally, on the basis of the worst-case situation, system-suitability tests were performed and acceptance limits for certain values were calculated.

Słowa kluczowe

EN

Plackett-Burman design; robustness; system-suitability tests; perindopril tert -butylamine; impurities; liquid chromatography

• Wydawca: University of Silesia in Katowice ; Akademiai Kiado
• Czasopismo: Acta Chromatographica
• Rocznik: 2010
• Tom: Vol. 22, no. 2
• Strony: 281--296
• Opis fizyczny: Bibliogr. 18 poz., rys., tab.

Twórcy

autor

Mašković M

• Medicines and Medical Devices Agency of Serbia, Belgrade Vojvode Stepe 458 Belgrade Serbia

autor

Jančić-Stojanović B

• Institute of Drug Analysis Faculty of Pharmacy Vojvode Stepe 450 Belgrade Serbia

autor

Malenović A.

• Institute of Drug Analysis Faculty of Pharmacy Vojvode Stepe 450 Belgrade Serbia

autor

Ivanović D.

• Institute of Drug Analysis Faculty of Pharmacy Vojvode Stepe 450 Belgrade Serbia

autor

Medenica M.

• Institute of Physical Chemistry Faculty of Pharmacy Vojvode Stepe 450 Belgrade Serbia

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