Yi Tao, Zhang Hao, Xie Jing, Xue Dan
West China School of Pharmacy, Sichuan University, No. 17 Section 3 Ren-Min-Nan-Lu Road, Chengdu, Sichuan 610041, P. R. China.
J Sep Sci. 2007 Aug;30(12):1973-8. doi: 10.1002/jssc.200700001.
A new procedure for the separation and isolation of Z-ligustilide from the roots of Angelica sinensis (AS) was developed, and the storage conditions for Z-ligustilide were optimized. Using the present procedure, Z-ligustilide was enriched by decomposing the Z-ligustilide dimers yielding Z-ligustilide and dissolving the polar impurities in hot water. Then, the crude Z-ligustilide was further purified by a semipreparative HPLC system. The spiked and nonspiked samples were used for the evaluation of the proposed procedure. Recoveries obtained varied from 86.2 to 90.7% and RSDs from 4.0 to 6.6%. The yield and purity of the isolated Z-ligustilide were found to be 4.57 mg/g and 99.6%, respectively. The results of stability tests have shown that the presence of oxidant contributes to Z-ligustilide degradation, therefore argon was chosen as a shielding gas for storage. The overall procedure is efficient and convenient which is considered suitable for the preparative separation of Z-ligustilide from AS.
开发了一种从当归根部分离和提纯Z-藁本内酯的新方法,并优化了Z-藁本内酯的储存条件。采用本方法,通过分解Z-藁本内酯二聚体得到Z-藁本内酯,并将极性杂质溶解在热水中,从而富集Z-藁本内酯。然后,通过半制备高效液相色谱系统进一步纯化粗制的Z-藁本内酯。加标和未加标样品用于评估所提出的方法。获得的回收率在86.2%至90.7%之间,相对标准偏差在4.0%至6.6%之间。分离得到的Z-藁本内酯的产率和纯度分别为4.57 mg/g和99.6%。稳定性测试结果表明,氧化剂的存在会导致Z-藁本内酯降解,因此选择氩气作为储存的保护气体。整个过程高效且方便,被认为适用于从当归中制备分离Z-藁本内酯。