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

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.

[Chemical constituents from hypoglycemic active part of Plantaginis Semen].

The chemical constituents of Plantaginis Semen with hypoglycemic effect was investigated in this paper. The previous results of the in vivo hypoglycemic effect showed that 60% ethanol extract of Plantaginis Semen decreased the levels of FBG and improved the glucose tolerance in high fat diet(HFD)-induced diabetic C57BL/6 mice. Then, in the present study, the above potential bioactive extract was separated and purified by silica gel, ODS, Sephadex LH-20 column chromatography, medium pressure liquid chromatography(MPLC)and preparative HPLC. The structures of isolated compounds were identified by physicochemical properties and spectral analyses. Eight compounds were obtained and identified as 4, 4a, 5, 7a-tetrahydro-7-(hydroxymethyl)cyclopenta[c]pyran-3(1H)-one(1), iridolactone(2), pedicularislacton(3), rehmaglutin C(4), geniposidic acid(5), p-hydroxylphenylglycerol(6), 1, 2-benzenediol-4-(2-hydroxyethyl)(7), and 3-buten-2-one-4-[3-(ß-D-glucopyranosyloxy)-4-hydroxyphenyl](8). Among them, compounds 1-5 were iridoids, and 6-8 were phenolic acids. Compound 1 was a new natural product, and compounds 2-4, 6 and 8 were isolated from the Plantaginaceae family for the first time.