Chiral and achiral liquid chromatographic separation of palonosetron hydrochloride and its related impurities utilizing two different stationary phases: Polysaccharide and alkyl amide columns

• Published in: Microchemical journal Vol. 168; p. 106398
• Main Authors: El-Wahab Mubarak, Marwa A., El-Bagary, Ramzia I., Abdul-Azim Mohammad, M., Abo-Talib, Nisreen F., Elkady, Ehab F.
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 01.09.2021
• Subjects: Bonus RP column; Chiralpak AD column; Enantioseparation; Palonosetron hydrochloride; Polar organic mode; Palonosetron hydrochloride; Chiralpak AD column; Enantioseparation; Bonus RP column; Polar organic mode
• ISSN: 0026-265X; 1095-9149
• DOI: 10.1016/j.microc.2021.106398

•Two LC methods were developed for determination of palonosetron and its impurities.•Method A: Chiral separation of palonosetron and its impurities using polar mode.•Method B: Green UPLC method separation of palonosetron and three of its impurities.•The two proposed methods were successfully validated according to ICH guidelines. In this work, two simple, sensitive and rapid liquid chromatographic (LC) methods were assessed; for the determination of palonosetron hydrochloride and its related impurities. Method A comprised stress study, chiral separation and quantification of palonosetron (PALO) and its six related impurities. The successful separation of PALO and its six related impurities was achieved using Chiralpak AD column (250 mm × 4.6 mm, 10 µm), in a polar organic (PO) mode. PALO was eluted using gradient mode, consisting of the mobile phase A: 0.1% diethylamine in acetonitrile, the mobile phase B: isopropanol. Method B is a green UPLC method to estimate PALO in the presence of three of its related impurities. Effective separation was carried out on Bonus RP column (100 mm × 4.6 mm, 1.8 µm), based on purified water- ethanol- triethylamine (75: 25: 0.1, v/v), pH 4.0 adjusted with 1 M acetic acid as the mobile phase. The validated methods showed excellent linearity (r2˃ 0.999) over the concentration ranges of 5.0–100.0 μg mL−1 and 0.1–10.0 μg mL−1 for method A and B, respectively. The values of the detection limit (LOD) and quantification limit (LOQ) of PALO and its six related impurities were found in the range of 0.014–0.032 μg mL−1 and 0.043–0.097 μg mL−1, respectively for method A, while for method B; they were found to be in the range of 0.08 and 0.1 μg mL−1, respectively. The optimized methods have been validated and found to be appropriate for quality control of PALO in its pharmaceutical dosage form.