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目的:分离鉴定双黄连粉针剂中的化学成分,丰富了双黄连粉针剂的物质基础,为阐释该制剂的致敏成分组和二次开发奠定了基础。方法:双黄连冻干粉通过大孔吸附树脂AB-8,反复硅胶柱色谱,反相ODS和制备HPLC等多种方法进行分离纯化,利用理化性质及MS,1D NMR,2D NMR等波谱学方法鉴定结构。结果:分离鉴定了7个化合物,分别是连翘脂素(1),千层纸素A(2),(+)-表松脂素-4’-O-β-D-吡喃葡萄糖苷(3),异落叶松脂醇(4),千层纸素A-7-O-β-D-葡萄糖醛酸苷甲酯(5),Chrysin-7-glucuronide methyl ester(6)和咖啡酸乙酯(7)。结论:化合物1~7均是首次从该复方得到,且化合物6和7在双黄连粉针的原料金银花、黄芩、连翘也未见报道。
OBJECTIVE: To separate and identify the chemical constituents in Shuanghuanglian injection and enrich the material basis of Shuanghuanglian injection, which lays the foundation for elucidating the allergenic constituents and the secondary development of this preparation. Methods: Shuanghuanlian freeze-dried powder was separated and purified by macroporous resin AB-8, repeated silica gel column chromatography, reverse phase ODS and preparative HPLC. The physicochemical properties and spectroscopic methods such as MS, 1D NMR and 2D NMR Identification structure. RESULTS: Seven compounds were isolated and identified as forsythiaside (1), melaleuca A (2), (+) - mesomatsin-4’-O-β-D-glucopyranoside 3, Chrysin-7-glucuronide methyl ester (6) and caffeic acid ethyl ester (4), melaleuca A-7-O-β-D-glucuronide methyl ester (7). CONCLUSION: Compounds 1 to 7 were obtained from this compound for the first time, and compounds 6 and 7 have not been reported on the raw materials of Shuanghuanglian, such as honeysuckle, skullcap and forsythia.