Isolation, Identification, and Characterization of an Unknown Impurity in Lovastatin EP

Chandrakant Belwal; Praveen Kumar Goyal; Anup Balte; Sandeep Kolhe; Kamlesh Chauhan; Ajay Singh Rawat; Anand Vardhan

doi:10.3797/scipharm.1305-04

Isolation, Identification, and Characterization of an Unknown Impurity in Lovastatin EP

Sci Pharm. 2013 Jul 1;82(1):43-52. doi: 10.3797/scipharm.1305-04. Print 2014 Jan-Mar.

Authors

Chandrakant Belwal¹, Praveen Kumar Goyal¹, Anup Balte¹, Sandeep Kolhe¹, Kamlesh Chauhan¹, Ajay Singh Rawat¹, Anand Vardhan¹

Affiliation

¹ Sterling Biotech Research Centre, Sterling Biotech Limited, Vadodara-391421, India.

Abstract

An unknown impurity in the fermentation-based drug substance lovastatin at 0.52 RRT was observed invariably in all batches when analyzed by HPLC as per the PhEur monograph. This impurity was isolated from the impurity-enriched sample using reversed-phase preparative HPLC and characterized by using spectroscopic (PMR, CMR, MASS, and UV) techniques as the structurally-related compound Monacolin-X, having the molecular formula C24H34O6 and the chemical name 2-methyl-3-oxobutanoic acid 1,2,3,7,8,8a-hexahydro-3,7-dimethyl-8-[2-(tetrahydro-4-hydroxy-6-oxo-2H-pyran-2-yl)ethyl]-1-naphthalenyl ester.

Keywords: Characterization; Chromatography; Identification; Isolation; Lovastatin; Prep HPLC.