Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities

Abstract

This paper describes the development and validation of a microemulsion liquid chromatography (MELC) method for simultaneous determination of perindopril tert-butylamine and its impurities in bulk active substances and the pharmaceutical dosage form of tablets. An appropriate resolution with reasonable retention times was obtained for a microemulsion containing 0.24% (w/v) butyl acetate, 0.30% (w/v) ethyl acetate, 2% (w/v) sodium dodecyl sulfate, 7.75% (w/v) n-butanol, and 20.0 mM potassium dihydrogen phosphate, the pH of which was adjusted to 3.70 with 85% orthophosphoric acid. Separations were performed on a Nucleosil 120-5 butyl modified (C4), 250 × 4 mm, 5 μm particle size silica column at 40°C, with a mobile phase flow rate of 1.25 mL/min. UV detection was performed at 254 nm. The established method was subjected to method validation, and required validation parameters were defined. Robustness testing, an important part of method validation, was performed as well. Since robustness validation can be conducted using different experimental designs, the Plackett-Burman design was applied due to its possibility of testing many factors at the same time. The validated MELC method was found to be suitable for the simultaneous determination of perindopril tert-butylamine and its impurities in pharmaceuticals.

Plackett-Burman design in robustness testing of liquid chromatographic method for determination of sodium-valproat

“…skrining vrsta dizajna. U literaturi se može naći primena Plaket-Burman dizajna [9][10][11], kao i punog faktorskog [12][13][14][15][16] i frakcionog faktorskog dizajna [17][18][19][20][21]. S obzirom da je u ovom radu primenjen Plaket-Burman dizajn, onda će on ovde i biti detaljnije opisan.…”

Analysis of isoquinoline alkaloids using chitosan‐assisted liquid–solid extraction followed by microemulsion liquid chromatography employing a sub‐2‐micron particle stationary phase

“…This separation mode, namely, microemulsion liquid chromatography (MELC), is exhibiting great potential in separation fields [6][7][8][9]. Currently, common chromatographic columns, such as Zorbax Extend-C 18 , Spherisorb C 18 , and Zorbax-Eclipse XDB-C 8 , with particle sizes of 3-5 m are widely used in conventional MELC [10]. Therefore, establishing an MELC system with sub-2-m particle size column is quite meaningful in the analysis of complex chemical constituents.…”

“…In recent years, ME used as a mobile phase in HPLC has been receiving increasing attentions. This separation mode, namely, microemulsion liquid chromatography (MELC), is exhibiting great potential in separation fields . Currently, common chromatographic columns, such as Zorbax Extend‐C 18 , Spherisorb C 18 , and Zorbax‐Eclipse XDB‐C 8 , with particle sizes of 3–5 μm are widely used in conventional MELC .…”