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Here we built a Raman fiber photometry, and created a highly selective non\u2010metallic Raman probe based on the triple\u2010recognition strategies of chemical reaction, charge transfer, and characteristic fingerprint peaks, for tracking and simultaneous quantitation of mitochondrial O<jats:sub>2<\/jats:sub><jats:sup>.\u2212<\/jats:sup>, Ca<jats:sup>2+<\/jats:sup> and pH at the same location in six brain regions of free\u2010moving animal upon hypoxia. It was found that mitochondrial O<jats:sub>2<\/jats:sub><jats:sup>.\u2212<\/jats:sup>, Ca<jats:sup>2+<\/jats:sup> and pH changed from superficial to deep brain regions upon hypoxia. It was discovered that hypoxia\u2010induced mitochondrial O<jats:sub>2<\/jats:sub><jats:sup>.\u2212<\/jats:sup> burst was regulated by ASIC1a, leading to mitochondrial Ca<jats:sup>2+<\/jats:sup> overload and acidification. Furthermore, we found the overload of mitochondrial Ca<jats:sup>2+<\/jats:sup> was mostly attributed to the influx of extracellular Ca<jats:sup>2+<\/jats:sup>.<\/jats:p>","DOI":"10.1002\/anie.202111630","type":"journal-article","created":{"date-parts":[[2021,12,1]],"date-time":"2021-12-01T03:52:49Z","timestamp":1638330769000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":33,"title":["Raman Fiber Photometry for Understanding Mitochondrial Superoxide Burst and Extracellular Calcium Ion Influx upon Acute Hypoxia in the Brain of Freely Moving Animals"],"prefix":"10.1002","volume":"61","author":[{"given":"Zhichao","family":"Liu","sequence":"first","affiliation":[{"name":"Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular Engineering East China Normal University  Dongchuan Road 500 Shanghai 200241 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