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Here, we first built a photoelectrochemical fiber cytometry with a tip size down to \u223c60\u00a0nm for real\u2010time collection of photoelectrochemical signals in brain slices. Meanwhile, a serotonin (5\u2010HT)\u2010selective photoelectrochemical probe kit was created using a dual\u2010recognition strategy, integrating aptamer binding\u2010induced selective recognition and photo\u2010conversion electron transfer processes. The developed two\u2010sensor probe kit enabled the monitoring of 5\u2010HT dynamics, with linear detection ranges covering two distinct concentration windows from nM to mM. Leveraging the high selectivity, reversible response, and precise spatial positioning capability of this tool, volume transmission\u2010associated 5\u2010HT dynamics were measured at the edges of open synaptic clefts and non\u2010synaptic varicosities in acute brain slices. The findings suggested that the P2X\n                    <jats:sub>2<\/jats:sub>\n                    receptor modulated extracellular ATP (eATP)\u2010induced 5\u2010HT dynamics at edges of both open synaptic and non\u2010synaptic varicosities. Moreover, the P2Y\n                    <jats:sub>12<\/jats:sub>\n                    receptor exerted a stronger regulatory effect on 5\u2010HT dynamics at the edge of open synaptic varicosities than at non\u2010synaptic varicosities under eATP stimulation.\n                  <\/jats:p>","DOI":"10.1002\/anie.8236222","type":"journal-article","created":{"date-parts":[[2026,9,26]],"date-time":"2026-09-26T15:32:12Z","timestamp":1790436732000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Photoelectrochemical Fiber Cytometry With 60\u00a0nm Tip Size for Measuring Serotonin Dynamics at Edges of Cleft and Varicosities"],"prefix":"10.1002","author":[{"given":"Yue","family":"Shangguan","sequence":"first","affiliation":[{"name":"Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular Engineering East China Normal University  Shanghai 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