The preparation of pre-alphacalcidol by high performance liquid chromatography

Abstract

Pre-alfacalcidol is an active substance, and the UV response of pre-alfacalcidol and alfacalcidol is different, there will be errors in the content determination process. The main reason is that pre-alfacalcidol is very unstable and easy to tautomerize with alfacalcidol at room temperature. Therefore, it is very necessary to control the content of pre-alfacalcidol and alfacalcidol when determining the content of alfacalcitol tablets. In order to fully study the quality of Alfacalcidol tablets, here, we reported a preparation method of pre-alfacalcidol. In this study, pre-alfacalcidol was prepared by directional degradation and purified by high performance liquid chromatography (HPLC) and its structure was identified by high resolution mass spectrometer (HRMS) and nuclear magnetic resonance (NMR). The preparation process is simple, and the cycle is short at a low cost with a high yield. The purity of pre-alfacalcidol is more than 95%, which can meet the requirements of standard products. At the same time, under the condition of high temperature preparation, the undamaged alfacalcidol can be collected and recovered, which greatly improves the availability and reduces the cost. In summary, this method has important significance to strictly control the quality of raw materials and preparations of alfacalcidol and improve the efficacy of alfacalcidol tablets.