Alkylresorcinols serve as critical biomarkers for whole-wheat grains, and their precise analysis is essential for authenticating and monitoring the quality of whole-wheat products. In this study, we developed a novel electrochemical sensor by using a disposable screen-printed electrode for the sensitive and selective detection of 5-heneicosylresorcinol (AR21). To enhance the sensor’s sensitivity and selectivity, multilayered Ti3C2Tx (m-Ti3C2Tx) nanomaterials were incorporated into the electrode in conjunction with molecularly imprinted polymers. Under optimized conditions, the sensor exhibited a linear detection range of 0.005 to 100 mg·L−1, with a detection limit of 3.98 μg·L−1 for AR21. Furthermore, the sensing platform demonstrated remarkable selectivity for AR21 when compared to structurally similar compounds, along with excellent reproducibility and stability. Validation studies with real wheat food samples confirmed the effectiveness of the proposed method, underscoring its potential as a rapid and portable solution for the assessment of whole-grain foods.
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