Dietary fiber and its quantitation in foods have been of significant interest in the nutrition community for over 50 years. A number of AOAC Official Methods of Analysis have been adopted for the analysis of dietary fiber and some of its fractions and components commensurate with the evolving discoveries of dietary fiber nutrition research. Quantitation of low-molecular-weight soluble dietary fiber (LMWSDF) has been difficult due to high solubility in a precipitating solvent mixture of four parts alcohol and one part water. AOAC Method 2001.03 effectively quantitates LWMSDF subsequent to gravimetric removal of high-molecular-weight dietary fiber using LC. However, deionization and concentration of the enzymatic digestate, necessary to assure accurate LC quantitation, requires substantial time and manual labor. A modification to the method and resulting method performance is presented that describes a means of simultaneously deionizing the digestate and quantitating the LMWSDF in a single LC injection, eliminating a number of time-consuming manual preparation steps.