School of Pharmacy, the Key Laboratory of Prescription Effect and Clinical valuation of State Administration of Traditional Chinese Medicine of China, Binzhou Medical University, Yantai, P. R. China.
J Sep Sci. 2019 Oct;42(19):3134-3140. doi: 10.1002/jssc.201900433. Epub 2019 Aug 14.
As a well-known traditional Chinese medicine, Ziziphi Spinosae Semen has been used for treating anxiety and insomnia for a long time. Spinosin, the main active C-glycoside flavonoid in Ziziphi Spinosae Semen, has attracted much attention because of its many pharmacological activities including strong hypnotic effects, anxiolytic-like effects, and so on. In the present work, high-purity spinosin was separated from Ziziphi Spinosae Semen using the HPD-300 resin followed by preparative high-performance liquid chromatography. The adsorption kinetics curve of spinosin on the HPD-300 resin was studied and fitted well by the pseudo-second-order equation. The adsorption isotherms were also constructed and low temperature favored the adsorption reaction. The separation parameters were optimized using dynamic adsorption and desorption tests. After a one-run treatment with HPD-300 resin, the concentration of spinosin increased 11.8-fold from 0.99 to 11.7% with a recovery yield of 80.4%. Furthermore, the purity of spinosin could surpass above 98% after separation by preparative high-performance liquid chromatography and recrystallization with a recovery yield of 72.6%. The developed method was effective and suitable for the large-scale preparation of spinosin. Moreover, it was confirmed that HPD-300 resin could enable good selection for the enrichment of flavonoids from different plants.
作为一种著名的中药，酸枣仁长期以来一直被用于治疗焦虑和失眠。酸枣仁中的主要活性 C-糖苷类黄酮——斯皮诺素，由于具有很强的催眠作用、抗焦虑样作用等多种药理活性而备受关注。在本工作中，采用 HPD-300 树脂从酸枣仁中分离出高纯度的斯皮诺素，然后通过制备高效液相色谱进行分离。研究了斯皮诺素在 HPD-300 树脂上的吸附动力学曲线，并通过拟二级方程拟合得很好。还构建了吸附等温线，低温有利于吸附反应。通过动态吸附和解吸试验优化了分离参数。经过 HPD-300 树脂一次处理，斯皮诺素的浓度从 0.99%提高到 11.7%，收率为 80.4%。此外，通过制备高效液相色谱和重结晶分离，斯皮诺素的纯度可超过 98%，收率为 72.6%。所开发的方法有效且适用于斯皮诺素的大规模制备。此外，还证实 HPD-300 树脂可以很好地选择从不同植物中富集黄酮类化合物。
