Following purification, the fractions of purified samples typically are analyzed to determine the relative purities of each fraction. We report a novel technique for performing post-purification analysis immediately after each preparative LC/MS run. The Single Pass Compound Purification and Analysis System (SPACPASS) samples and stores a representative aliquot from the fraction while it is being collected. Demonstrated for '1:1' fraction collections, this method of fraction purity assessment streamlined sample processing by reducing post-purification sample handling. For 97% of the collected fractions, this technique provided relative purities to within +/-5% when compared with more traditional post-purification analysis.