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To improve the capacity to probe volatile chemical substances in the atmosphere, we designed an unmanned aerial vehicle system for volatile organic compound (VOC) monitoring and sampling. This environmental monitoring unmanned aerial vehicle (EMUAV) platform was equipped with a photoionization detector for continuous VOC monitoring and searching in a pollution air mass. Furthermore, a multifunction airborne microVOC sampler was loaded for sampling. An airbag and absorption tube were applied to collect air samples for further analyzing in the laboratory by GC-FID/MS or TD-GC/MS. By comparing the aerial samples derived from the microVOC sampler with the samples collected at a similar height to a building roof for chemical compositions, the sampling conditions, such as the sampling port location and sampling method, were optimized to ensure the representativeness of the air samples. The results of the sample comparison experiment showed that both the airbag method and the adsorption method could recover 70–130% for most VOC species. Through the aerial measurements, the advantages of this EMUAV system were demonstrated. Therefore, the developed EMUAV system would have immeasurable potential in the field of environment monitoring. [ABSTRACT FROM AUTHOR]