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Per- and polyfluoroalkyl substances (PFAS) accumulate in the human body, presenting heightened risks to infants during critical development. Assessing safety in infant formula requires more than measuring total PFAS; it demands distinguishing structural isomers, such as the linear and branched forms of PFOS, which often possess different toxicological profiles. Conventional LC-MS workflows frequently lack the resolution to separate these molecules without impractical chromatographic runtimes. This study addresses the challenge of resolving isomeric PFAS species in complex infant formula matrices at EU-regulated levels. We demonstrate a rapid workflow coupling LC-MS with high-resolution ion mobility (HRIM). This orthogonal gas-phase separation distinguishes branched and linear isomers based onmolecular shape, providing accurate collision cross section (CCS) values to improve characterization confidence.