A Validated LC Method for the Determination of Chiral Purity of (S) - (-) - 3-Tert Butylamino 1,2, Propane Diol) : A key Raw material of Timolol maleate

Vinayak T. Vele; Sandesh M Patil; Rupesh V. Palav; Ramki Iyer; Mohan A Chandavarkar

Volume : VIII, Issue : IV, April - 2018

A Validated LC Method for the Determination of Chiral Purity of (S) - (-) - 3-Tert Butylamino 1,2, Propane Diol) : A key Raw material of Timolol maleate

Vinayak T. Vele, Sandesh M Patil, Rupesh V. Palav, Ramki Iyer, Mohan A Chandavarkar

Abstract :

A simple and accurate normal phase liquid chromatographic method was developed for the

determination of chiral purity of (S) – (–) – 3–Tert Butylamino 1,2, Propane Diol, S–enantiomer used as key starting raw material in the manufacturing of timolol maleate bulk drug.

Chromatographic separation between (S) – (–) – 3–Tert Butylamino 1,2, Propane Diol and its opposite enantiomer (R) – (–) – 3–Tert Butylamino 1,2, Propane Diol, R–enantiomer was achieved using a Chiralpak IC column using a mobile phase containing n–hexane, ethanol, formic acid and diethylamine (70:30:0.1:0.1 v/v/v/v). The resolution between the two enantiomers was found to be more than 5.0. The limit of detection (LOD) and limit of quantification (LOQ) of the R–enantiomer was 7.5 and 25.0 μg mL–1, respectively, for 20 μL injection volume. The percentage

recoveries of the R–enantiomer ranged from 96.4 to 98.1 in the samples of (S) – (–) – 3–Tert Butylamino 1,2, Propane Diol. The test solution and mobile phase was observed to be stable up to 24 h after the preparation. The developed method was validated as per International Conference on Harmonization guidelines in terms of LOD, LOQ, precision, linearity, accuracy, robustness and ruggedness.