Robust optimization of gradient RP HPLC method for simultaneous determination of ivabradine and its eleven related substances by AQbD approach

• Autorzy: Tomić Jovana , Djajić Nevena , Agbaba Danica , Otašević Biljana , Malenović Andjelija , Protić Ana

Identyfikatory

DOI

10.1556/1326.2021.00885

• Języki publikacji: EN

Abstrakty

EN

This paper is aimed at developing a gradient elution reversed-phase high-performance liquid chromatography (RP-HPLC) method for the separation of a complex mixture composed of ivabradine and its eleven impurities, in a reasonable timeframe. In order to obtain a robust and reliable HPLC method for separation of this mixture, Analytical Quality by Design (AQbD) was applied. This approach demonstrated to be useful in development of a long lasting life cycle methods. Four chromatographic variables were defined as key method parameters (KMPs) and optimized towards the analytical target profile (ATP). Designated KMPs were initial and final amount of acetonitrile in the mobile phase, pH value of the aqueous phase and gradient time, while resolutions of critical peak pairs were denoted as critical method attributes (CMAs). Relationships between KMPs and CMAs were obtained with the aid of Design of Experiments (DoEs) methodology among which Box-Behnken design (BBD) was employed to gain valid mathematical models. Obtained mathematical equations were used to construct the Design Space (DS) and select reliable optimal separation conditions. They included 11% (v/v) and 34% (v/v) of initial and final amount of acetonitrile, respectively, as well as 45 min of gradient elution time and 20 mM ammonium acetate as aqueous mobile phase with pH set to 7.35. The possibility to separate the diastereoisomers of impurity X was also evaluated. It was demonstrated that this separation could not be achieved in gradient elution mode within the defined variable domains and in a reasonable time span. The developed method was validated according to ICH Q2 (R1) guideline and met all the required criteria.

Słowa kluczowe

EN

ivabradine; gradient elution RP-HPLC method; Box-Behnken design; analytical quality by design

• Wydawca: University of Silesia in Katowice ; Akademiai Kiado
• Czasopismo: Acta Chromatographica
• Rocznik: 2022
• Tom: Vol. 34, no. 1
• Strony: 1--11
• Opis fizyczny: Bibliogr. 36 poz., rys., tab.

Twórcy

autor

Tomić Jovana

• Department of Pharmaceutical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11 152, Belgrade, Serbia

autor

Djajić Nevena

• Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11 221Belgrade, Serbia

autor

Agbaba Danica

• Department of Pharmaceutical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11 152, Belgrade, Serbia

autor

Otašević Biljana

• Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11 221Belgrade, Serbia

autor

Malenović Andjelija

• Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11 221Belgrade, Serbia

autor

Protić Ana

• Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11 221Belgrade, Serbia

• https://orcid.org/0000-0002-6304-1913

Bibliografia

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Uwagi

Opracowanie rekordu ze środków MEiN, umowa nr SONP/SP/546092/2022 w ramach programu "Społeczna odpowiedzialność nauki" - moduł: Popularyzacja nauki i promocja sportu (2022-2023).