HPLC-DAD及HPLC-MS研究干燥工艺对中药粗榧化学成分的影响  

Effect of Drying on the Chemical Constituents of Cephalotaxus Sinensis Extract by HPLC-DAD and HPLC-MS

作　　者：李伟[1] 禹玉洪[1] 戴荣继[1] 李良[1] 孟薇薇[1] 邓玉林[1] 

机构地区：[1]北京理工大学生命科学与技术学院

出　　处：《精细化工》2007年第4期350-354,共5页Fine Chemicals

摘　　要：用高效液相色谱-二极管阵列检测器及高效液相色谱-质谱联用技术,发现常压及减压干燥能使粗榧提取物中两个主要的化合物（1号峰和2号峰）发生降解。减压干燥后两个化合物分别减少了20.2%和45.6%,常压干燥后,两个化合物均检测不到。与干燥前相比,减压干燥和常压干燥使3号峰面积分别增加了1.90倍和5.74倍。1-3号峰均具有特征性的黄酮化合物的两个紫外吸收带（240-280 nm和300-400 nm）,被推测为黄酮化合物,质谱研究推测1-2号峰发生了苷键断裂生成3号峰。用AB-8大孔吸附树脂,葡聚糖凝胶LH-20,反相硅胶（ODS）柱色谱分离纯化得到1-3号峰的3个化合物,对其进行了红外和核磁测定,鉴定出芹菜素-5-O-α-L-吡喃鼠李糖基（1→4）-β-D-吡喃葡萄糖苷和芹菜素-5-O-α-L-吡喃鼠李糖基（1→4）-6″-O-乙酰基-β-D-吡喃葡萄糖苷两个黄酮苷,干燥过程使它们苷键断裂生成了苷元芹菜素（3号峰）。Two major components （peaks 1,2 ）in the extract of Cephalotaxus sinensis （Rehd et Wile）Li broke up during drying, which was investigated by techniques of high-performance liquid chromatography with photodiode array detection （HPLC -DAD ） and high-performance liquid chromatography-electrospray ionization tandem mass spectrometry （ HPLC - MS）. The two components decreased by 20. 2% , 45.6% , respectively, after drying in vacuo, and they were not observed after drying under atmospheric pressure. The area of peak 3 increased by 1.90- and 5.74-fold, respectively, after drying in vacuo and under atmospheric pressure. It is inferred that the three peaks are flavones having two characteristic UV absorbance bands （240 - 280 nm and 300 - 400 nm） of flavones, and peaks 1 - 2 produce peak 3 by bond cleavage during drying. The extract was subjected successively to column chromatography on AB -8 macroporous absorbent resin, Sephadex LH -20 and reverse-phase silica gel （ODS） to afford three compounds. They are identified as apigenin-5-O-[ α-L- rhamnopyranosyl- （ 1→4 ） -β-D-glucopyranoside ] （ peak 1 ）, apigenin-5-O- [ α-L-rhamnopyranosyl- （ 1 → 4 ）-6-O-β-D-acetylglucopyranoside] （peak 2） and apigenin（ peak 3） by IR and NMR analysis, and the two flavone glycosides （ peaks 1,2） produce apigenin, the aglycone, after drying.

关 键 词：中华粗榧 高效液相色谱-二极管阵列检测器 高效液相色谱-质谱 芹菜素 芹菜素-5-O-α-L-吡喃鼠李糖基(1→4)-β-D-吡喃葡萄糖苷 芹菜素-5-O-α-L-吡喃鼠李糖基(1→4)-6″-O-乙酰基-β-D-吡喃葡萄糖苷 

分 类 号：R284.1[医药卫生—中药学]