A simple, new, and sensitive spectrophotometric technique for the determination of methyldopa was presented in this research article. The suggested technique includes reacting metoclopramide with NaNO2 in the presence of hydrochloric acid to produce diazonium salt, and then the drug methyldopa reacts with the diazonium salt to produce a yellow azo dye. The maximum wavelength of the dye was 458 nm. This method is effectively used for the determination of methyldopa in different pharmaceutical formulations. It has been found that there are no significant interactions between common excipients and pure methyldopa. The results were processed statistically, and compared with those obtained from officially approved methods, they were found to be reasonable.