Wang Zhuwei, Zhang Lixia, Sun Yuqing
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, P.R. China.
J Chromatogr Sci. 2005 May-Jun;43(5):249-52. doi: 10.1093/chromsci/43.5.249.
A method for the isolation, purification, and determination of eleutheroside E in Acanthopanax giraldii Harms, collected in the Sichuan province (China), is established. The water extraction of A. giraldii Harms is pre-isolated using macroporous adsorption resin (D-101) and a C18 solid-phase extraction cartridge, and the enriched extract is purified to give eleutheroside E (syringaresinol-di-O-beta-D-glucoside; liriodendrin) by semipreparative reversed-phase high-performance liquid chromatography. Structure identification is performed by a comparison of IR, 1H-NMR, 13C-NMR, and electrospray ionization-mass spectrometric data with the literature. The final purity of the compound is 97%. Quantitative determination of eleutheroside E in A. giraldii Harms is performed on a Zorbax SB C18 (150- x 4.6-mm i.d., 5 microm) column. The linear range of eleutheroside E is 4.85-194 mg/L (r = 0.9998), and the average recovery is 99.6-101%. The developed method is simple, reproducible, and easy to operate. It is useful for the evaluation of Acanthopanax giraldii Harms.
建立了一种从采自中国四川省的红毛五加中分离、纯化并测定刺五加苷E的方法。红毛五加的水提取物先用大孔吸附树脂(D - 101)和C18固相萃取柱进行预分离,富集后的提取物通过半制备反相高效液相色谱法纯化得到刺五加苷E(紫丁香树脂醇 - 二 - O - β - D - 葡萄糖苷;鹅掌楸苷)。通过将红外光谱(IR)、1H - 核磁共振(1H - NMR)、13C - 核磁共振(13C - NMR)和电喷雾电离质谱数据与文献进行比较来进行结构鉴定。该化合物的最终纯度为97%。在Zorbax SB C18(内径150×4.6 mm,粒径5微米)柱上对红毛五加中的刺五加苷E进行定量测定。刺五加苷E的线性范围为4.85 - 194 mg/L(r = 0.9998),平均回收率为99.6 - 101%。所建立的方法简单、可重复且易于操作。它对红毛五加的评价具有实用价值。