The recognition and separation of polar chiral compounds are important technological challenges in separation science. Taking full advantage of the intrinsically chiral environment and multiple interactions featured by macrocycles, we designed the first example of porous methylated cyclodextrins-containing polymers (MP-CDPs) with three-dimensional (3D) chiral channels. The enantioselective recognition of (R)/(S)-1-phenylethylamine mixtures was realized with enantiomer excess (e.e.) >73% in only 3 min by using MP-CDPs as the adsorbent. The obtained MP-CDPs also serve as highly efficient liquid chromatographic stationary phases for separation of polar chiral compounds. The stationary phase can separate racemic alcohols and acids successfully. These chiral compounds can be separated within 8 min under normal-phase mode, and the resolution (R_S) range from 1.76 to 3.00. Molecular simulations suggest that chiral recognition is a cooperative interaction based on multiple effects such as host-guest interaction, H-bond and size selection. These findings will provide novel chiral stationary phases for recognition and separation of polar chiral compounds in the fields of separation science and pharmaceutical industry.

极性手性化合物的识别和分离是分离科学中的重要技术挑战。充分利用固有手性环境和大环化合物所具有的多种相互作用，我们设计了具有三维（3D）手性通道的含多孔甲基化环糊精的聚合物（MP-CDP）的第一个实例。（R）/（S）-1-苯基乙胺混合物的对映选择性识别是通过对映体过量（ee。）使用MP-CDP作为吸附剂，仅3分钟即可> 73％。所得的MP-CDP还可以用作高效液相色谱固定相，用于分离极性手性化合物。固定相可以成功分离外消旋的醇和酸。这些手性化合物可在8分钟内下正相模式分离，并且分辨率（ř_小号）的范围从1.76至3.00。分子模拟表明，手性识别是一种基于多种效应的协同相互作用，例如宿主-客体相互作用，氢键和大小选择。这些发现将为分离科学和制药工业领域中极性手性化合物的识别和分离提供新颖的手性固定相。