The present invention relates to novel crystalline forms of Epirubicin hydrochloride "SBL-1", "SBL-2" and "SBL-3" in particular "SBL-3", which is useful as an anti-cancer chemotherapeutic drug. The present invention also provides process for preparing novel crystalline forms of Epirubicin hydrochloride "SBL-1", "SBL-2" and "SBL-3" in particular "SBL-3", which are distinct and reproducible in a consistent manner.