Published:  Aug 31, 2018DOI: 10.7324/JAPS.2018.8805
Objective: Enantiomeric resolution of racemic 1-(4-Methoxybenzyl)-1,2,3,4,5,6,7,8-octahydroisoquinoline, a key starting material in the synthesis of the antitussive agent dextromethorphan hydrobromide. Material and method: Chiral liquid chromatographic method is developed and enantiomers are resolved on a Chiralpak ID-3 column using gradient mode of elution. Mobile phase A and B containing a mixture of 0.1% diethylamine in acetonitrile and 0.1% diethylamine in methanol respectively are optimized with the timed programme. The flow rate is 1.0 mL/minute and the column temperature was maintained at 40°C. Ultraviolet detection was performed at 280 nm wavelength and the injection volume was 20 μL. Results: The resolution between the enantiomers is found to be more than 2.5. The developed method is extensively validated and proved to be robust. The limit of detection and limit of quantification of unwanted (R)-enantiomer is found to be 0.0075% and 0.025% with respect to test concentration, respectively. The percentage recovery of (R)-enantiomer is ranged from 88.6 to 106.6 in (S)-(-)-1-(4-Methoxybenzyl)-1,2,3,4,5,6,7,8- octahydroisoquinoline sample solution. Conclusion: The proposed method is found to be suitable and accurate for the quantitative determination of (R)-enantiomer in the key starting material of the dextromethorphan hydrobromide bulk drugs.
Anerao A, Solase V, More A, Pradhan N. Separation, Quantification and Control of Enatiomers of the Key Starting Material of Dextromethorphan Hydrobromide. J App Pharm Sci, 2018; 8(08): 032-038.
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