Intercalation compounds of organic anions into layered double hydroxides (LDH) are synthesized by the coprecipitation route. X-ray diffraction data reveal that the intercalated terephthalate (TP), naphthalene-2,6-disulfonate (NA26), and anthraquinone-2,6-disulfonate (AQ26) are arranged with their molecular planes perpendicular to the hydroxide layer. HPLC data show that 26.2% of TP and 73.8% of AQ26 are cointercalated, whereas NA26 is not intercalated into the Zn/Al-LDH. These results indicate the possibility of a molecular recognition ability of Zn/Al-LDH. The molecular recognition ability of intercalation into Zn/Al-LDH is in the order AQ26 > TP >> NA26.