Department of Pharmacognosy with Medicinal Plant Unit, Medical University of Lublin, Lublin, Poland.
J Sep Sci. 2013 Aug;36(16):2611-4. doi: 10.1002/jssc.201300407. Epub 2013 Jul 17.
High-performance counter-current chromatography was successfully used for the isolation and purification of terpenoid compounds from the essential oil of Pimpinella anisum L. A two-phase solvent system composed of n-heptane/methanol/ethyl acetate/water (5:2:5:2, v/v/v/v) was suitable for the purification of linalool, terpinen-4-ol, α-terpineol, p-anisaldehyde, while n-heptane/methanol (1:1, v/v) was used for the isolation of anethole and foeniculin. A scale-up process from analytical to preparative was developed. Additionally, a stepwise gradient elution was applied and instead of two different runs, 40 min each, one 80 min separation was performed; although the time of separation remains the same, it was possible to repeat the efficiency even if the water-containing mobile phase was changed to a nonaqueous system. The obtained essential oil, as well as purified compounds, was analyzed by GC. A total of 0.64 mg of linalool, 0.52 mg of terpinen-4-ol, 0.10 mg of α-terpineol, 0.62 mg of p-anisaldehyde, 15 mg of anethole, and 2.12 mg of foeniculin were obtained from 210 mg of the essential oil of P. anisum L. in a short time with purities of 99, 98, 94, 93.54, 93, and 93.6%, respectively.
高效逆流色谱成功用于从茴芹精油中分离和纯化萜类化合物。两相溶剂系统由正庚烷/甲醇/乙酸乙酯/水（5:2:5:2，v/v/v/v）组成，适用于纯化芳樟醇、萜品-4-醇、α-萜品醇、对甲氧基苯甲醛，而正庚烷/甲醇（1:1，v/v）则用于分离茴香脑和茴香脑素。从分析规模到制备规模都开发了一种放大工艺。此外，还应用了分步梯度洗脱，而不是两个不同的运行，每个运行 80 分钟，只需进行一次 80 分钟的分离；虽然分离时间保持不变，但即使将含水的流动相改为非水体系，也可以重复效率。所得精油以及纯化化合物均通过 GC 进行分析。从 210 毫克 P. anisum L. 的精油中，在短时间内获得了 0.64 毫克芳樟醇、0.52 毫克萜品-4-醇、0.10 毫克α-萜品醇、0.62 毫克对甲氧基苯甲醛、15 毫克茴香脑和 2.12 毫克茴香脑素，纯度分别为 99%、98%、94%、93.54%、93%和 93.6%。
