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A nanocomposite consists of AuNPs, GQD, and poly(L‐lysine) was prepared for highly sensitive electrochemical determination of dopamine (DA) and serotonin (5‐HT) neurotransmitters which are of vital importance in neurological disorders. The P(L‐Lys) GQD was successfully obtained a one‐step co‐electrodeposition of GQD and L‐Lys on the PGE. The electrochemical behaviors of DA and 5‐HT were analyzed via DPV and CV. LOD values for DA and 5‐HT were calculated as 0.03 μM and 0.017 μM, respectively. Also, the DA and 5‐HT contents were determined at the PGE/AuNPs/P(L‐Lys)‐GQD in fetal bovine serum samples and pharmaceutical formulations, and high recovery values were obtained.

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