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A cross-reactive sensor array consisting of polyion complexes (PICs) between anionic enzymes and poly(ethylene glycol)-modified (PEGylated) polyamines has been used to identify the source of mammalian sera. Although the catalytic activity of enzymes was inhibited by PIC formation with PEGylated polyamines, the subsequent addition of sera caused enzyme releases from PICs through competitive interactions between PICs and serum proteins, generating unique response patterns of changes in the enzyme activity. Linear discriminant analysis of the obtained patterns enabled the discrimination of five sera from different mammalian sources.