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In this work, two detection methods of solid-phase extraction–high-performance liquid chromatography (SPE-HPLC) and quartz crystal microbalance (QCM) were established, based on a surface molecularly imprinted polymer material (MIP). The material can be used as a selective solid-phase extraction filler and as a coating for sensitive quartz crystal microbalances by virtue of the polyhydroxy structure of grafted silicon spheres together with the network structure from cross-linked polymerization. The adsorption properties of the prepared MIP were analysed by dynamic and static adsorption tests, and the experimental conditions for SPE-HPLC and QCM analysis were optimized. Under the optimal conditions, the linear range of MIP-SPE-HPLC for the detection of carbaryl was 0.5–60 μg L
−1
(
R
2
= 0.99913), and the detection limit was 0.0573 μg L
−1
. The proposed QCM sensor displayed a linear relationship between the frequency shift and the concentration of carbaryl ranging from 5 to 80 μg L
−1
with a low detection limit of 0.6845 μg L
−1
(signal-to-noise ratio, S/
N
= 3). Through a series of experiments, it was shown that the prepared MIP has good adsorption and selectivity for carbaryl, and the MIP-based HPLC and QCM sensor can be applied to the detection of actual food samples.