Enantiopurity Assessment of Chiral Switch of Ondansetron by Direct Chiral HPLC
2017
Kannappan, Valliappan | Kanthiah, Selvakumar
A simple, selective, robust, and rapid enantiospecific HPLC method was developed and optimized for simultaneous determination of ondansetron enantiomers. The chiral separation was performed on Chiralpak AS-3R analytical column (150 mm × 4.6 mm i.d., 3 µm). AD-optimal mixture design methodology was employed to evaluate the influence of solvent mixtures on retention factor of first peak (k ₁), resolution between enantiomers (Rs₁,₂) and runtime (tR₂). Solvent mixtures are delivered at 1.5 mL min⁻¹ flow rate, and enantiomeric peaks were detected at 222 nm. Experiments were carried out, and results were analyzed by the two-component mix plot graph of the design software. The mobile phase containing methanol/water/diethylamine (85/15/0.1% v/v/v) leads to a best possible combination adequate retention (k ₁ = 1.4), enantiomeric resolution (Rs₁,₂ = 2.9) in shorter runtime (3.5 min). The proposed method was validated according to ICH guidelines and found to be linear, sensitive, selective, precise, and accurate. Furthermore, the pertinence of this developed method was established by analyzing two commercially available tablets: Emeset-8 (racemic mixture) and Zordil-4 (R-ondansetron). Good agreement was found between the assay results and the label claim of the marketed formulations by showing good % recovery and %CV. The study resulted in a better chromatographic system for chiral impurity profiling of ondansetron chiral switch.
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