山荷叶中木脂素的薄层扫描测定

STUDIES ON THE TLC SCANNING DETERMINATION OF LIGNANS IN DIPHYLLEIA SINENSIS LI

在高效硅胶薄层板上,用二氯甲烷-乙醚分离了山荷叶中6种苯基四氢萘丁内酯类木脂素:鬼臼酮、异苦鬼臼酮、苦鬼臼酮、苦鬼臼素、鬼臼毒素、4’-去甲基鬼臼毒素和2种苯基萘丁内酯:去氢鬼臼素、山荷叶素。用2.5％硫酸铈铵的20％硝酸溶液喷雾显色,氨气薰数分钟后,薄层扫描法测定,各木脂素的线性范围在0.48～2.52μg,并用此法测定了不同产地的山荷叶及相近属植物鬼臼和山荷叶中木脂素的含量,方法简便、快速、灵敏度高。

A simple, sensitive and accurate method for the separation and determination of the lignans: podophylltoxone (Ⅰ), isopicropodophyllone (Ⅱ), picropodophyllone (Ⅲ), dehydropodo-phyUotoxin (Ⅳ), picropodophyllin (Ⅴ), podophyllotoxin (Ⅵ), 4′-demethylpodophyllotoxin (Ⅶ)and diphyllin (Ⅷ) is described. The sample solution was applied at a point 1 cm from the bottom edge of the HPTLC silica gelplate (10 cm × 10 cm), dichloromethane--diethyl ether (4:1) was used as the developing solvent.The plate was saturated for 30 min and then developed twice for 9. 5 cm using ascending technique. The plate was sprayed with 2. 5% ammonium ceric sniphate--20% nitric acid and toasted for 15 minat 120°C, then fumigated with ammonia solution for 20 min at room temperature to intensify thecolor. The spots were scanned with a Shimadzu CS-930 TLC scanner. The contents of eight lignans inDiphylleia sinensis was calculated by comparison with standards spotted on the same plate. The standard curves were linear in the ren of 0. 48～2. 52 μg for the eight lignans. The method has been applied to the analysis of various samples and can be used for the quality control ofsinensis, podophyllum and dysosma preparations used in clinic.