Open AccessDevelopment and Validation of Three Potential Genotoxic Impurities by Liquid Chromatography Single Quad Mass Detector in Iomeprol
Author(s) -
Rayala Rama Rao,
Gundapaneni Ravi Kumar,
Vadde Megha Vardhan,
B. Veeraswami
Publication year - 2021
Publication title -
journal of pharmaceutical research international
Language(s) - English
Resource type - Journals
ISSN - 2456-9119
DOI - 10.9734/jpri/2021/v33i47a33071
Subject(s) - repeatability , chromatography , detection limit , chemistry , formic acid , calibration curve , analytical chemistry (journal) , high performance liquid chromatography , impurity , mass spectrometry , organic chemistry
A liquid chromatography with single quadrupole mass detection method was developed for the determination of potential genotoxic impurities (PGIs) in the Iomeprol active pharmaceutical ingredient. Chromatographic separation was achieved on an Agilent Eclipse plus C8 column (100 mm x 2.1 mm x 1.8 μm) with 0.1% formic acid in water as mobile phase A and acetonitrile as mobile phase B in gradient elution mode at a 0.1 mL/min. Executed validation summary demonstrated that the mass detection method had highly sensitive and selective. A linear calibration curve (correlation coefficient, r> 0.999) was attained at the concentration range of 0.1-125 ppm for three PGI’s. The Limit of Detection of Imp-A, Imp-B and Imp-C in drug substance of Iomeprol is 0.05 ppm. The accuracy was confirmed by calculated recoveries (98.4-101.5%). The precision was tested at three levels: injection repeatability, analysis repeatability and intermediate precision. The calculated relative standard deviations were within the specification. The developed method was able to quantitate all three PGI’s at a concentration level of 1 µg/mL.