The application of metal–organic frameworks (MOFs) as SERS‐active platforms in multiplex volatile organic compounds (VOCs) detection is still unexplored. Herein, we demonstrate that MIL‐100 (Fe) serves as an ideal SERS substrate for the detection of VOCs. The limit of detection (LOD) of MIL‐100(Fe) for toluene sensing can reach 2.5 ppm, and can be even further decreased to 0.48 ppb level when “hot spots” in between Au nanoparticles are employed onto MIL‐100 (Fe) substrate, resulting in an enhancement factor of 1010. Additionally, we show that MIL‐100(Fe) substrate has a unique “sensor array” property allowing multiplex VOCs detection, with great modifiability and expandability by doping with foreign metal elements. Finally, the MIL‐100(Fe) platform is utilized to simultaneously detect the different gaseous indicators of lung cancer with a ppm detection limit, demonstrating its high potential for early diagnosis of lung cancer in vivo.

The application of metal-organic frameworks (MOFs) as SERS-active platforms in multiplex volatile organic compounds (VOCs) detection is still unexplored. Herein, we demonstrate that MIL-100 (Fe) serves as an ideal SERS substrate for the detection of VOCs. The limit of detection (LOD) of MIL-100(Fe) for toluene sensing can reach 2.5 ppm, and can be even further decreased to 0.48 ppb level when "hot spots" in between Au nanoparticles are employed onto MIL-100 (Fe) substrate, resulting in an enhancement factor of 10 10. Additionally, we show that MIL-100(Fe) substrate has a unique "sensor array" property allowing multiplex VOCs detection, with great modifiability and expandability by doping with foreign metal elements. Finally, the MIL-100(Fe) platform is utilized to simultaneously detect the different gaseous indicators of lung cancer with a ppm detection limit, demonstrating its high potential for early diagnosis of lung cancer in vivo.

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