Ti‐Doping Activates Adjacent Zr Sites in Bimetallic MOFs for Cooperative Phospholipid Removals in Human Biomonitoring

ABSTRACT The interference of phospholipids in serum poses a critical bottleneck for nontargeted human biomonitoring of chemical hazards. Here, we report a Ti‐doping strategy to activate adjacent Zr sites in a bimetallic Zr/Ti metal‐organic framework (B‐Zr/Ti MOF) for cooperative and efficient phospholipid removal. By precisely engineering the Ti content, the optimal B‐Zr/Ti MOF achieves near‐complete removal of major phospholipid subclasses while maintaining high recoveries (>50%) for over 500 diverse chemical hazards, even at trace levels (10 ng mL ^{− 1} ). Combined XPS, FT‐IR, and DFT calculations reveal that Ti incorporation modulates the local electronic environment, converting adjacent Zr sites into highly active Lewis acid centers that synergistically anchor phosphate headgroups via inner‐sphere coordination. When integrated into a nontargeted LC‐HRMS workflow, this material dramatically reduces matrix effects and expands detectable feature coverage. This work establishes bimetallic node engineering as a powerful strategy to overcome matrix interference in exposomics and precision biomonitoring.