Finally, the cocrystallization of INH and SYA was preliminarily detected after the liquid-assisted grinding using isoproponal as solvent. On this basis, by employing the resulting solid as seeds, INH-SYA cocrystal, consisting of INH and SYA in a 1:1 molar ratio, was successfully obtained by crystallization technique in a mixture solvent system including isopropanol, methanol and ethyl acetate (1:3:1, v/v/v). Then the cocrystal was thoroughly characterized by the following SCXRD, PXRD and DSC methods.