Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, China; University of Chinese Academy of Sciences, Beijing, China.
Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Jun 15;1118-1119:70-77. doi: 10.1016/j.jchromb.2019.04.039. Epub 2019 Apr 18.
Polar compounds are abundant in the water decoction of Traditional Chinese Medicines (TCMs) and possess important biological activities. However, purifying these compounds has faced great difficulties largely due to poor retention and insufficient selectivity. To solve this problem, an offline orthogonal 2-D RPLC coupled with hydrophilic interaction chromatography (HILIC) method was developed to achieve purification of polar compounds from Caulis Polygoni Multiflori. A polar-copolymerized XAqua C18 column and a zwitterionic Click XIon column exhibited satisfactory retention and separation for polar compounds. Therefore, they were adopted to construct the offline 2-D LC system. Furthermore, the method presented a high orthogonality, which was calculated to be 72%. The XAqua C18 column was used in the first dimension to fractionate the 5.1 g polar fraction with a recovery of 85% within 10 h. In the second dimension, three representative fractions were purified using the Click XIon column. Finally, three compounds with purity higher than 95% were identified for the first time from this plant. This offline 2-D RPLC/HILIC method was shown to be an effective approach to purifying polar compounds from Caulis Polygoni Multiflori.
极性化合物在中药水提物中含量丰富，具有重要的生物活性。然而，由于保留性差和选择性不足，这些化合物的纯化一直面临很大的困难。为了解决这个问题，开发了一种离线正交 2-D RPLC 与亲水相互作用色谱（HILIC）联用的方法，以从何首乌中纯化极性化合物。极性共聚的 XAqua C18 柱和两性离子 Click XIon 柱对极性化合物表现出良好的保留和分离性能。因此，它们被用于构建离线 2-D LC 系统。此外，该方法具有较高的正交性，计算值为 72%。XAqua C18 柱用于第一维，在 10 小时内以 85%的回收率对 5.1 g 的极性馏分进行分离。在第二维，使用 Click XIon 柱对三个代表性馏分进行纯化。最后，首次从该植物中鉴定出三种纯度高于 95%的化合物。这种离线 2-D RPLC/HILIC 方法被证明是一种从何首乌中纯化极性化合物的有效方法。
