Antisolvent crystallization is the most common method to study solvent effects on polymorphic crystallization. L‐Histidine (L‐his) served as a model substance. Acetonitrile, acetone, and methanol were selected as antisolvents, with water as solvent. The formation of L‐his polymorphs in antisolvent crystallization as a function of supersaturation, antisolvent volume fraction, and temperature was studied. The solubility of polymorph A of L‐his decreased with increasing volume fraction of antisolvent and increased with higher temperature. The metastable polymorph B of L‐his was obtained at higher antisolvent volume fraction and supersaturation. At lower antisolvent volume fraction and supersaturation, a mixture of polymorphs A and B was detected.