The invention belongs to the interdisciplinary field of inorganic chemistry and organic chemistry and discloses preparation of a macrocyclic molecule-modified nano silica capillary chromatographic column. Nano silica is modified first with silylation reagent APTS, macrocyclic molecules are then reacted with dichloride oxalate, separating and purifying are carried out to obtain macrocyclic molecule acyl chloride, and the macrocyclic molecule acyl chloride is then reacted with the modified nano silica to obtain the macrocyclic molecule-modified nano silica; the macrocyclic molecule-modified nano silica is charged into a capillary chromatographic column through a column charging pump, nitrogen flushing is carried out, and the temperature 280 DEG C is held for 12 h to obtain the capillary chromatographic column. The capillary chromatographic column prepared herein has an important application prospect in terms of separation, purification and chiral enantiomer separation.