The
combined application of nanozymes and surface-enhanced Raman
scattering (SERS) provides a promising approach to obtain label-free
detection. However, developing nanomaterials with both highly efficient
enzyme-like activity and excellent SERS sensitivity remains a huge
challenge. Herein, we proposed one-step synthesis of Mo2N nanoparticles (NPs) as a “two-in-one” substrate,
which exhibits both excellent peroxidase (POD)-like activity and high
SERS activity. Its mimetic POD activity can catalyze the 3,3′,5,5′-tetramethylbenzidine
(TMB) molecule to SERS-active oxidized TMB (ox-TMB) with high efficiency.
Furthermore, combining experimental profiling with theory, the mechanism
of POD-like activity and SERS enhancement of Mo2N NPs was
explored in depth. Benefiting from the outstanding properties of Mo2N NPs, a versatile platform for indirect SERS detection of
biomarkers was developed based on the Mo2N NPs-catalyzed
product ox-TMB, which acts as the SERS signal readout. The feasibility
of this platform was validated using glutathione (GSH) and target
antigens alpha-fetoprotein antigen (AFP) and carcinoembryonic antigen
(CEA) as representatives of small molecules with a hydroxyl radical
(·OH) scavenging effect and proteins with a low Raman scattering
cross-section, respectively. The limits of detection of GSH, AFP,
and CEA were as low as 0.1 μmol/L, 89.1, and 74.6 pg/mL, respectively.
Significantly, it also showed application in human serum samples with
recoveries ranging from 96.0 to 101%. The acquired values based on
this platform were compared with the standard electrochemiluminescence
method, and the relative error was less than ±7.3. This work
not only provides a strategy for developing highly active bifunctional
nanomaterials but also manifests their widespread application for
multiple biomarkers analysis.