Microchip isotachophoresis for green and sustainable pharmaceutical quality control: Method validation and application to complex pharmaceutical formulations

• Published in: Journal of Chromatography A 2024-08, Vol.1729, p.465055, Article 465055
• Main Authors: Ďuriš, Marta, Hradski, Jasna, Szucs, Roman, Masár, Marián
• Format: Article
• Language: English
• Subjects: Active pharmaceutical ingredient; Counterion; Green analytical chemistry; Microchip isotachophoresis; Pharmaceutical analysis
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2024.465055

•Microchip isotachophoresis methods for pharmaceutical quality control developed.•Universal methods validated in accordance with the ICH guideline.•The greenness of the proposed methods evaluated.•Active ingredients and counterions determined in six commercial formulations. Universal microchip isotachophoresis (μITP) methods were developed for the determination of cationic and anionic macrocomponents (active pharmaceutical ingredients and counterions) in cardiovascular drugs marketed in salt form, amlodipine besylate and perindopril erbumine. The developed methods are characterized by low reagent and sample consumption, waste production and energy consumption, require only minimal sample preparation and provide fast analysis. The greenness of the proposed methods was assessed using AGREE. An internal standard addition was used to improve the quantitative parameters of μITP. The proposed methods were validated according to the ICH guideline. Linearity, precision, accuracy and specificity were evaluated for each of the studied analytes and all set validation criteria were met. Good linearity was observed in the presence of matrix and in the absence of matrix, with a correlation coefficient of at least 0.9993. The developed methods allowed precise and accurate determination of the studied analytes, the RSD of the quantitative and qualitative parameters were less than 1.5% and the recoveries ranged from 98 to 102%. The developed μITP methods were successfully applied to the determination of cationic and anionic macrocomponents in six commercially available pharmaceutical formulations.