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Despite exhaled human breath having enabled noninvasive diabetes diagnosis, selective acetone vapor detection by fluorescence approach in the diabetic range (1.8–3.5 ppm) remains a long‐standing challenge. A set of water‐resistant luminescent metal‐organic framework (MOF)‐based composites have been reported for detecting acetone vapor in the diabetic range with a limit of detection of 200 ppb. The luminescent materials possess the ability to selectively detect acetone vapor from a mixture comprising nitrogen, oxygen, carbon dioxide, water vapor, and alcohol vapor, which are prevalent in exhaled breath. It is noteworthy that this is the first luminescent MOF material capable of selectively detecting acetone vapor in the diabetic range via a turn‐on mechanism. The material can be reused within a matter of minutes under ambient conditions. Industrially pertinent electrospun luminescent fibers are likewise fabricated alongside various luminescent films for selective detection of ultratrace quantities of acetone vapor present in the air. Ab initio theoretical calculations combined with in situ synchrotron‐based dosing studies uncovered the material's remarkable hypersensitivity toward acetone vapor. Finally, a freshly designed prototype fluorescence‐based portable optical sensor is utilized as a proof‐of‐concept for the rapid detection of acetone vapor within the diabetic range. [ABSTRACT FROM AUTHOR]