[Study on preparation method of reference substance of aristolactam â -deoxyriboside adducts].

ABSTRACT

A two-step synthetic process of bromination and cross-coupling with aristololactam Ⅰ as raw material was successfully developed. Three aristolactam Ⅰ-deoxyriboside adducts, namely AAⅠ-dA, AAⅠ-dG, and AAⅠ-dC were obtained after a sequential procedure of impurity removal and purification in four different solvents. The yield of the two-step reaction can reach 90%, and the purity of the product is more than 98%, which can meet the requirements of qualitative and quantitative analyses as traditional Chinese medicine chemical reference products. The process has been proven to have good repeatability and scalability, and it features a concise preparation procedure, efficient purification, and high yield and purity, requiring no chromatographic separation. Compared with pre-vious methods, the newly developed process has significant advantages and is suitable for the preparation of chemical reference products of aristolactam Ⅰ-deoxyriboside adducts. This process provides technical support for the preparation of reference products of aristolactam Ⅰ-deoxyriboside adducts and a solid material basis for the related toxicological research.