A VALIDATED LC METHOD FOR THE DETERMINATION OF CHIRAL PURITY OF (R)-3-((1-METHYLPYRROLIDIN-2-YL) METHYL)-5-(METHYLSULFONYLMETHYL)-1H-INDOLE: A KEY RAW MATERIAL OF ELITRIPTAN HYDROBROMIDEAbstract
A simple and accurate normal phase liquid chromatographic method was developed for the determination of chiral purity of (R)-3-((1-methylpyrrolidin-2-yl) methyl)-5-(methylsulfonylmethyl)-1H-indole, R-isomer used as key starting raw material in the manufacturing of Elitriptan hydrobromide bulk drug. Chromatographic separation between (R)-3-((1-methylpyrrolidin-2-yl) methyl)-5-(methylsulfonylmethyl)-1H-indole and its opposite isomer (S)-3-((1-methylpyrrolidin-2-yl) methyl)-5-(methylsulfonylmethyl)-1H-indole, S -isomer was achieved using a Chiralpak IA column using a mobile phase containing n-hexane, ethanol, isopropyl alcohol and trifluoro acetic acid (98:1.5:0.5:0.1 v/v/v/v). The resolution between the two isomers was found to be more than 2.0. The limit of detection (LOD) and limit of quantification (LOQ) of the S – isomer was 0.15 and 0.5 μg mL-1, respectively, for 10 μL injection volume. The percentage recoveries of the S-isomer ranged from 96.5 to 105.3 in the samples of (R)-3-((1-methylpyrrolidin-2-yl) methyl)-5-(methylsulfonylmethyl)-1H-indole. 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.
M. Sarat, P. Murali Krishna and C. Rambabu*
Acharya Nagarjuna University, Nagarjuna Nagar-522510, Guntur dist, Andhra Pradesh, India
03 May, 2012
23 July, 2012
29 August, 2012
01 September, 2012