Zhang Jing, Jin Yu, Liu Yanfang, Xiao Yuansheng, Feng Jiatao, Xue Xingya, Zhang Xiuli, Liang Xinmiao
Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China.
J Sep Sci. 2009 May;32(9):1401-6. doi: 10.1002/jssc.200800729.
Two-dimensional preparative multi-channel parallel high performance liquid chromatography was successfully applied for the first time to isolate and purify alkaloids from Corydalis yanhusuo. The experiments were performed in off-line mode using the same preparative chromatographic column with pH 3.5 in the first and pH 10.0 in the second separation dimension. In the preparative process, UV-triggered fraction collection was used in the first dimension while UV and MS-triggered collection were used in the second dimension for reasons of sensitivity and complementarity. Two pure compounds and nine fractions were obtained in the first dimension. Then two representative fractions were further purified in the second dimension and six pure compounds were obtained. The results demonstrated that this procedure is an effective approach for the preparative isolation and purification of alkaloids from Corydalis yanhusuo. Based on the different pH values of the mobile phase in this method, it is also suitable for the preparative isolation and purification of other compounds from TCMs which are sensitive to the pH of the solutions. Moreover, this method will be a promising tool for the purification of low content compounds from natural products.
二维制备型多通道平行高效液相色谱首次成功应用于从延胡索中分离纯化生物碱。实验采用离线模式,在第一分离维度使用pH 3.5的同一制备色谱柱,在第二分离维度使用pH 10.0的同一制备色谱柱。在制备过程中,由于灵敏度和互补性的原因,第一维度采用紫外触发馏分收集,第二维度采用紫外和质谱触发收集。在第一维度获得了两种纯化合物和九个馏分。然后在第二维度对两个代表性馏分进一步纯化,获得了六种纯化合物。结果表明,该方法是从延胡索中制备分离纯化生物碱的有效方法。基于该方法中流动相不同的pH值,它也适用于从对溶液pH敏感的中药中制备分离纯化其他化合物。此外,该方法将是用于从天然产物中纯化低含量化合物的有前途的工具。