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The accurate quantification of neurotransmitter molecules is an indispensable means to reveal the physiological mechanisms of neuro movement in molecular level.However,existing detection strategies cannot fully meet practical needs,and the on-site and in vivo detection of neurotransmitters in brain remains a great challenge.Here,we report the development of a near infrared light responsive photoelectrochemical (PEC) detection method for in vivo quantification of neurotransmitter dopamine in mouse brain.Under guidance of density function theory calculations,a combination strategy of non-metal cation doping and defect engineering is introduced to rationally design the micro-photoelectrodes with excellent biocompatibility and stability and implements the in vivo PEC detection of dopamine in mouse brain.It opens up a new way for the accurate in vivo detection of biomolecules and allows researchers to make novel inquiries for long-standing questions in a new way.