Zan Ke, Guo Li-Nong, Zheng Jian, Ma Shuang-Cheng
National Institutes for Food and Drug Control, Beijing 100050, China.
Zhongguo Zhong Yao Za Zhi. 2016 Jan;41(1):101-105. doi: 10.4268/cjcmm20160120.
In order to isolate and purify the reference compounds and improve the quality standard of ethnic medicine of Radix of Cynanchum otophyllum, the ethanol extracts were isolated by column chromatography onsilica gel, C₁₈ reverse-phase silica gel, and semi-preparative HPLC. Twelve compounds were isolated and their structures were elucidated as 2,4-dihydroxy-6-methoxyphenylethanone(1), 4,6-dihydroxy-2-methoxyphenylethanone(2), p-hydroxyacetophenone(3), baishouwubenzophenone(4), 2,4-dihydroxyacetophenone(5), 2,5-dihydroxyacetophenone(6), otophylloside A(7),otophylloside B(8), caudatin-3-O-β-D-cymaropyranosyl-(1→4)-β-D-digitoxopyranoside(9),caudatin-3-O-β-D-glucopyranosyl-(1→4)-β-D-oleandropyranosyl-(1→4)-β-D-cymaropyranosyl-(1→4)-β-D-digitoxopyranoside(10),qingyangshengenin-3-O-β-D-oleandropyranosyl-(1→4)-β-D-cymaropyranoside(11),caudatin-3-O-β-D-oleandropyranosyl-(1→4)-β-D-cymaropyranosyl-(1→4)-β-D-cymaropyranoside(12) on the basis of spectral analysis. Compounds 1 and 2 were isolated from the genus Cynanchum for the first time, and compounds 3-4, 9-12 were obtained from this plant for the first time.These compounds are main active components of Radix of C.otophyllum and can be used as reference substances for the quality control of this ethnic medicine.
为了分离纯化对照品，提高青阳参民族药的质量标准，采用硅胶柱色谱、C₁₈反相硅胶柱色谱和半制备高效液相色谱法对乙醇提取物进行分离。分离得到12个化合物，通过波谱分析鉴定其结构分别为2,4 - 二羟基 - 6 - 甲氧基苯乙酮(1)、4,6 - 二羟基 - 2 - 甲氧基苯乙酮(2)、对羟基苯乙酮(3)、白首乌二苯酮(4)、2,4 - 二羟基苯乙酮(5)、2,5 - 二羟基苯乙酮(6)、青阳参苷A(7)、青阳参苷B(8)、牛皮消苷元 - 3 - O - β - D - 磁麻吡喃糖基 - (1→4) - β - D - 洋地黄毒吡喃糖苷(9)、牛皮消苷元 - 3 - O - β - D - 葡萄糖吡喃糖基 - (1→4) - β - D - 夹竹桃吡喃糖基 - (1→4) - β - D - 磁麻吡喃糖基 - (1→4) - β - D - 洋地黄毒吡喃糖苷(10)、青羊参苷元 - 3 - O - β - D - 夹竹桃吡喃糖基 - (1→4) - β - D - 磁麻吡喃糖苷(11)、牛皮消苷元 - 3 - O - β - D - 夹竹桃吡喃糖基 - (1→4) - β - D - 磁麻吡喃糖基 - (1→4) - β - D - 磁麻吡喃糖苷(12)。化合物1和2为首次从鹅绒藤属植物中分离得到，化合物3 - 4、9 - 12为首次从该植物中获得。这些化合物是青阳参的主要活性成分，可作为该民族药质量控制的对照品。
