| Summary: | As new psychoactive substances (commonly known as “the third generation drugs”) have characteristics such as short-term emergence, rapid updating, and great social harmfulness, there is a large gap in the development of their detection methods. Herein, graphite oxide (GO) was first prepared and immobilized with a reversible addition-fragmentation chain transfer (RAFT) agent, then a new psychoactive substance (4-MEC) was chosen as a template, and then the surface RAFT polymerization of methacrylamide (MAAM) was carried out by using azobisisobutyronitrile (AIBN) as an initiator and divinylbenzene (DVB) as a cross-linker. After the removal of the embedded template, graphene oxide modified by molecularly imprinted polymers (GO-MIPs) was finally obtained. Owing to the specific imprinted cavities for 4-MEC, the satisfactory selectivity and stability of the GO-MIP nanocomposite have been demonstrated. The GO-MIP nanocomposite was then used to fabricate the electrochemical sensor, which displayed a high selectivity in detecting 4-MEC over a linear concentration range between 5 and 60 μg mL<sup>−1</sup> with a detection limit of 0.438 μg mL<sup>−1</sup>. As a result, the GO-MIPs sensor developed an accurate, efficient, convenient, and sensitive method for public security departments to detect illicit drugs and new psychoactive substances.
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