A highly sensitive fluorometric method for determining sulfite in wine is reported. N-(9-Aciridinyl)maleimide (NAM) reacted with the sulfite in wine quantitatively and gave strong fluorescent derivatives. The determinations were conducted by batch and high-performance liquid chromatographic methods. Sulfite contents in wine by NAM methods and the conventional methods showed good accordance. The sample size could be reduced to less than 1/10,000 by the NAM methods.