Zhao Weiquan, Yang Guang, Zhong Fanyi, Yang Nan, Zhao Xin, Qi Yunpeng, Fan Guorong
Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai, P.R. China; Shanghai Key Laboratory for Pharmaceutical Metabolite Research, Shanghai, P.R. China; Shanghai Research Centre for Drug (Chinese Materia Medica) Metabolism, Shanghai, P.R. China.
J Sep Sci. 2014 Sep;37(17):2300-6. doi: 10.1002/jssc.201400270. Epub 2014 Jul 14.
Silymarin extracted from Silybum marianum (L.) Gaertn consists of a large number of flavonolignans, of which diastereoisomeric flavonolignans including silybin A and silybin B, and isosilybin A and isosilybin B are the main bioactive components, whose preparation from the crude extracts is still a difficult task. In this work, binary-column recycling preparative high-performance liquid chromatography systems without sample loop trapping, where two columns were switched alternately via one or two six-port switching valves, were established and successfully applied to the isolation and purification of the four diastereoisomeric flavonolignans from silymarin. The proposed system showed significant advantages over conventional preparative high-performance liquid chromatography with a single column in increasing efficiency and reducing the cost. To obtain the same amounts of products, the proposed system spends only one tenth of the time that the conventional system spends, and needs only one eleventh of the solvent that the conventional system consumes. Using the proposed system, the four diastereoisomers were successfully isolated from silymarin with purities over 98%.
从水飞蓟（Silybum marianum (L.) Gaertn）中提取的水飞蓟素由大量黄酮木脂素组成，其中包括水飞蓟宾A和水飞蓟宾B、异水飞蓟宾A和异水飞蓟宾B等非对映异构黄酮木脂素是主要生物活性成分，从粗提物中制备这些成分仍然是一项艰巨的任务。在这项工作中，建立了无样品环捕集的双柱循环制备高效液相色谱系统，该系统通过一个或两个六通切换阀交替切换两根色谱柱，并成功应用于从水飞蓟素中分离纯化四种非对映异构黄酮木脂素。与传统的单柱制备高效液相色谱相比，该系统在提高效率和降低成本方面具有显著优势。为了获得相同量的产物，该系统花费的时间仅为传统系统的十分之一，消耗的溶剂仅为传统系统的十一分之一。使用该系统，成功从水飞蓟素中分离出四种非对映异构体，纯度超过98%。
