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Numerous attempts have been made to replace commercial bulky gas chromatography (GC) systems with compact GC systems for monitoring volatile organic compounds in indoor air. However, recently developed compact GC systems are still too bulky in terms of user convenience, portability, and on-site analysis. Hence, an advanced miniaturization of compact GC systems is needed. Importantly, the small and high-performance gas pretreatment chip devices should be developed for compact GC systems. This paper reports the development of a metal–organic framework (MOF)-coated hybrid micro gas chromatography column chip (hybrid GC chip) capable of preconcentration and separation on harmful volatile organic compounds at low-concentration in one single chip device. The hybrid GC chip, 2 cm × 2 cm in size, was fabricated using a microelectromechanical systems process. The synthesized MOF-5 particles were coated on the inner wall of the fabricated hybrid GC chip and acted as an adsorbent and a stationary phase. The developed hybrid GC chip afforded high preconcentration factors with 1033–1237 and high separation resolutions with 3.8–13.3. The developed column showed good performance as a gas preconcentrator and separation column, and is the first device to perform both roles in one single chip device. [ABSTRACT FROM AUTHOR]