目的 研究大花红景天Rhodiola crenulata干燥根及根茎的化学成分.方法 利用反复硅胶柱色谱、中压柱色谱等方法分离纯化;采用ESI-MS、1H-NMR、13C-NMR等现代波谱技术进行结构鉴定.结果 从大花红景天醋酸乙酯部位分离得到14个化合物,分别鉴定为3,5-二羟基-3',4',7-三甲氧基黄酮(1)、3,5,7,3'-四羟基黄酮(2)、5,4 '-二羟基-7,3 '-二甲氧基黄酮(3)、山柰酚(4)、山柰酚-3-O-β-D-吡喃葡萄糖苷(5)、山柰酚-3-O-α-L-吡喃鼠李糖苷(6)、小麦黄素(7)、小麦黄素-7-O-β-D-吡喃葡萄糖苷(8)、槲皮素(9)、槲皮素-3-O-β-D-吡喃葡萄糖苷(10)、槲皮素-3-O-α-L-吡喃鼠李糖苷(11)、草质素-3-O-β-D-吡喃葡萄糖苷(12)、草质素-7-O-β-D-吡喃葡萄糖苷(13)、草质素-7-O-α-L-吡喃鼠李糖苷(14).结论 化合物1～3为首次从红景天属植物中分离得到,5～6、8、10～13为首次从该植物中分离得到.

Objective To establish a method for directional separation of dehydrotumulosic acid from the extracts of Guizhi Fuling Capsule with molecular imprinting technique(MIT). Methods Molecular imprinting polymer(MIP) was prepared by sol-gel process with dehydrotumulosic acid as molecular template to study the absorption property. The dehydrotumulosic acid was achieved from Guizhi Fuling Capsule by one-step separation with polymer as filler. The structure of dehydrotumulosic acid was identified on the basis of the spectral data and physicochemical property. Results The maximum binding capacity(Qmax) of MIP was 9.10 mg/g measured by Scatchard equation and the purity of dehydrotumulosic acid was 90.76% by HPLC. Conclusion The established MIT for the directional separation of dehydrotumulosic acid from Guizhi Fuling Capsule is simple and benefit to reducing the solvent use during the separation process, which could offer a novel method for the separation and purification of dehydrotumulosic acid.

This study was aimed to establish a separation method for neochlorogenic acid reference substances from Lonicera japonica. Refined neochlorogenic acid inL. japonica water extract was separated and concentrated by HPD200A macroporous resin, which was isolated and purified by medium-low-pressure preparative chromatography and determined by HPLC. The structure was identified by various spectroscopic data including ESI-MS,1H-NMR and13C-NMR. The results showed that the optimal purification technology conditions were as follows: washed with 5BV of water, collected elution, concentration, drying; neochlorogenic acid crude products were eluted with acetonitrile-0.5% formic acid solution (10:90) with the flow rate of 20 mL·min-1; and the detection wavelength was 326 nm. The contents of the prepared neochlorogenic acid reached to 98.86% and the yield was 89.1%. It was concluded that the method was effective for the preparation of neochlorogenic acid with high purity. It can be used to prepare the reference substances for quantitative analysis and content determination of Chinese materia medica.

OBJECTIVETo study the anti-complementary phenolic acids from Lonicera japonica.METHODThe anti-complementary activity-directed isolation was carried out with the hemolysis test as guide. All isolation was evaluated for their in vitro anti-complementary activities. The structures were identified by various spectroscopic data including ESI-MS, 1H-NMR, 13C-NMR data.RESULTFourteen compounds were isolated from the EtOAc fraction of L. japonica extracts, including 8 phenolic acids: 5-O-caffeoylquinic acid (1), chlorogenic (2), 4-O-caffeoylquinic acid (3), 3,5-di-O-caffeoylquinic acid (4), 4,5-di-O-caffeoylquinic acid (5), 3,4-di-O-caffeoylquinic acid (6), caffeic acid (7) and methyl caffeate acid (8); 3 iridoids: secologanoside (9), sweroside (10) and secoxyloganin (11); and 3 flavonoids: luteolin (12), quercetin (13) and kaempferol (14). Compounds 1-9 and 11-14 showed anti-complementary activity in different extents and 3,5-di-O-caffeoylquinic acid (4) exhibited the most significant activity against the classical pathway.CONCLUSIONCompound 14 is obtained from this plant for the first time, phenolic acids are the main anti-complementary constituents of L. japonica and 3,5-di-O-caffeoylquinic acid(4) is a potential complement inhibitor with strong activity, which worthy to be studied further in the future.

目的 建立从金银花Lonicera japonica中分离制备高质量分数异绿原酸A、B和C的方法.方法 采用D-101大孔树脂、中低压制备色谱分离制备金银花中异绿原酸A、B和C单体,根据理化性质和波谱数据鉴定其结构.结果 分离制备的异绿原酸A、B和C质量分数分别为98.7％、99.2％和97.6％.结论 该方法经济、简单、快速,可用于制备高质量分数的异绿原酸A、B和C.