Aspectrophotometric method is presented for the determination of Ascorbic Acid and Analgin in prescence of each other using a first dervative spectrophotometry. By measuring the absolute value of the first-order contribution of both drugs in prescence of each other. The concentration of both drugs can be calculated without interference from each other. The method was proved using synthetic mixtures of Ascorbic Acid and Analgin in prescence of each other.