A method using Raman spectroscopy was recently developed for the determination of the degree of substitution of succinate in waxy maize starch. In this paper it is demonstrated that the method can be generalized to a wide range of starches of different amylose contents and botanical origins. Raman calibration sets were used to form regression equations for five types of succinylated starches, that is, waxy, regular, and two high-amylose maize samples (47 and 66% amylose, respectively) and wheat. The derived calibration curves can be used to find the degree of substitution in samples with unknown levels of succinylation. The Raman calibration lines had linear correlation coefficients of 0.995 or better and enable the fast and nondestructive determination of the degree of substitution of succinate for different types of starches with minimal sample preparation. Also discussed is the potential utility of Raman spectroscopy to simultaneously determine the degree of substitution of succinate and amylose content, using previously determined calibration curves developed for the amylose content of maize starches.