Research

October 29, 2011

A simple method for isolation and structural identification of arctigenin from Saussurea medusa Maxim. by preparation chromatography and single crystal X-ray diffraction

Arctigenin was successfully isolated and purified from the crude extract of Saussurea medusa Maxim. by automatic flash preparation chromatography (AFPC). Chromatographic separation was performed with a gradient elution of (A) petroleum ether and (B) acetone.

The qualitative analysis was accomplished with thin layer chromatography (TLC) under the following conditions: petroleum ether-acetone (5:3, v/v) was used as a developing agent and improved Dragendorff's reagent as a coloring agent at 105°C. The rate of flow is about 0.38, the spot showed reddish yellow. The purity of arctigenin is 99.371%, which was determined by Agilent 1200 high performance liquid chromatograph (HPLC). Its structure was identified by single crystal X-ray diffraction. Arctigenin crystallized in the orthorhombic system, space group P21/n; The unit cell dimensions are as follows: a=9.5649(11) ?, b=10.0929(12) ?, c=20.133(2) ?, α=90°, β=90°,? =90°, Z=4.

Figure 1. (a) The molecular structure of arctigenin, with the
atom-numbering scheme. (b) A partial packing diagram of
arctigenin, hydrogen bonds are shown as dashed lines. (c) A
packing diagram of arctigenin.

Additional Information:
1 Author Information:Ruitao Yu1, Zhong Liu2,4, Ruixue Yu3, Huaigang Zhang1, Yun Shao1, Lijuan Mei1, Yanduo Tao1*
Correspondence:  taoyanduo1963@163.com
2 Published : 18 March 2011, Journal of Medicinal Plants Research Vol. 5(6), pp. 979-983.

A simple method for isolation and structural identification of arctigenin from Saussurea medusa Maxim. by preparation chromatography and single crystal X-ray diffraction.pdf