Ochratoxin
A (OTA), a toxic mycotoxin in contaminated cereal-based
food, poses a great challenge to human health worldwide. Hence, fabricating
sensitive and robust chemo/biosensors for OTA in the field of food
safety is still highly desired. Herein, we developed an upconversion
luminescence and surface-enhanced Raman scattering (UCL–SERS)
dual-mode aptasensor for the sensitive detection of OTA by using upconversion
nanoparticles (UCNPs) as a luminescence label, gold nanourchins (GNUs)
as an enhancing substrate, and the organic dye TAMRA as a quencher
and Raman reporter. The “turn-on” dual-mode aptasensor
was assembled through the hybridization of complementary DNA-conjugated
UCNPs (cDNA–UCNPs) and TAMRA-aptamer-modified GNUs (TAMRA-Apt-GNUs),
which produced both weak UCL and SERS signals. Upon the addition of
OTA, this aptasensor disintegrated to release cDNA–UCNPs due
to the preferential combination of the aptamer with OTA, resulting
in the recovery of UCL. In addition, conformational alteration of
the aptamer shortened the spatial distance between TAMRA and GNU,
generating a high SERS signal. Under optimal conditions, this dual-mode
aptasensor achieved low detection limits of 3.2 pg/mL (0.01–100
ng/mL) with the UCL modality and 8.6 pg/mL (0.01–50 ng/mL)
with the SERS modality. This aptasensor was further applied to detect
OTA in spiked beer samples with recoveries of 95.2–103% for
UCL and 92.4–108% for SERS. Compared with the single-mode sensor,
the proposed aptasensor had more detection flexibility with two alternative
support instruments, improved detection accuracy, and good complementarity
by combining the merits of the two signals. We envision that this
biosensor would hold great application prospects in monitoring biological
contaminants.