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

Mašković M, Jančić-Stojanović B, Malenović A., Ivanović D., Medenica M.

Acta Chromatographica

2010

Vol. 22, no. 2

281--296

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.

Validation of an analytical procedure for simultaneous determination of hydrochlorothiazide, lisinopril, and their impurities

Ivanović D., Medenica M., Jančić B., Knežević N., Malenović A., Milić J.

Acta Chromatographica

2007

No. 18

143-156

The main objective of the work discussed in this paper was evaluation of a chromatographic method for simultaneous determination of hydrochlorothiazide (HCTZ), lisinopril (L), and their impurities in pharmaceuticals. Chlorothiazide (CTZ) and disulfonamide (DSA), as potential impurities in hydrochlorothiazide, and diketopiperazine (DKP), as an impurity of lisinopril, were analyzed. The chromatographic behaviour of these substances on different columns was studied using mobile phases of different polarity. The optimum separations were achieved by gradient elution on a 4.6 mm × 20 mm, 3.5 µm particle size, C18 column. The mobile phase was a gradient prepared by mixing 7:93 (v/v) acetonitrile–25 mM potassium dihydrogen phosphate, pH 5, and 50:50 (v/v) acetonitrile–25 mM potassium dihydrogen phosphate pH 5 in different ratios. The flow rate was 1.0 mL min-1. UV detection was performed at 215 nm. Methylparaben was used as internal standard. The method was validated for selectivity, linearity, precision, and accuracy. The limits of detection, LOD, and quantification, LOQ, were determined experimentally. Because of its speed and accuracy the method can be used for quality-control analysis.