The volatile components of Camellia luteoflora Y.K.Li were detected by GC-MS. The differences in volatile composition of Camellia luteoflora Y.K.Li from organs by different extraction methods were compared. The essential oil of C. luteoflora was extracted by ultrasonic-assisted extraction (UAE) and head space solid-phase micro-extractions (HS-SPME), respectively. Their components were analyzed by gas chromatography-mass spectrometry (GC-MS), and further identified by NIST08.LIB standard mass spectrometry library. The peak area normalization method was used to quantitatively analyze these compounds. A total of 137 volatile components were detected in flowers and leaves, and 121 were identified. The 74 compounds were identified in flowers, including 15 terpenoids, 1 steroids, 11 aromatic compounds and 46 aliphatic compounds. The content of linalool (16.71%) was the highest. The 72 compounds were identified in leaves, including 23 terpenoids, 2 steroids, 14 aromatic compounds and 33 aliphatic compounds. Trans-2-hexenal (20.63%) had the highest content. There were 25 compounds both in flowers and leaves, including linalool, trans-2-hexenal and hexanal, which accounted for 44.82% of flowers and 47.69% of leaves, respectively. In this work, a variety of volatile components with pharmacological activities and attracting insect pests were identified in C. luteoflora, which laid a foundation for understanding the volatile components of C. luteoflora and provided a theoretical basis for pests control and relative product development and utilization.