Abstract: Abstract By the hydrolysis of pyridoxal-5-phosphate Schiff bases, pyridoxal-5-phosphate was prepared in a crystalline form without any further purification. Pyridoxal-5-phosphate Schiff bases were prepared in good yields by the phosphorylation of pyridoxal Scruff bases and were easily purified by alkali-acid reprecipitation. The pyridoxal-5-phosphate thus obtained was demonstrated to be identical with an authentic sample by a study of its UV, IR, and NMR spectra.