Indirect reversed‐phase high‐performance liquid chromatographic and direct thin‐layer chromatographic enantioresolution of (R,S)‐Cinacalcet |
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Authors: | Ravi Bhushan Rituraj Dubey |
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Affiliation: | Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667, India |
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Abstract: | Enantioresolution of the calcimimetic drug (R,S)‐Cinacalcet was achieved using both indirect and direct approaches. Six chiral variants of Marfey's reagent having l ‐Ala‐NH2, l ‐Phe‐NH2, l ‐Val‐NH2, l ‐Leu‐NH2, l ‐Met‐NH2 and d ‐Phg‐NH2 as chiral auxiliaries were used as derivatizing reagents under microwave irradiation. Derivatization conditions were optimized. Reversed‐phase high‐performance liquid chromatography was successful using binary mixtures of aqueous trifluoroacetic acid and acetonitrile for separation of diastereomeric pairs with detection at 340 nm. Thin silica gel layers impregnated with optically pure l ‐histidine and l ‐arginine were used for direct resolution of enantiomers. The limit of detection was found to be 60 pmol in HPLC while in TLC it was found to be in the range of 0.26–0.28 µg for each enantiomers. Copyright © 2010 John Wiley & Sons, Ltd. |
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Keywords: | (R,S)‐cinacalcet reversed‐phase HPLC Marfey's reagent l‐histidine l‐arginine impregnated TLC |
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