This chapter presents comprehensive information on applications and developments of supercritical fluid extraction (SFE) technique in plant oils and herbal volatile components analysis. Supercritical carbon dioxide (SC‐CO
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) is widely used for extraction and isolation of volatile and essential oil of plants. SFE possesses valuable advantages in extraction of various analytes, especially nonpolar compounds, from plant matrices. Meanwhile, some modifications such as the usage of modifiers make this technique applicable for the extraction of polar targets as well. SFE in herbal field is used for the extraction of a wide range of analytes including food, agricultural agents, pharmaceuticals, cosmetics, and pesticides. This chapter aims to review, from plant oil analysis standpoint, recent advances in the use of SC‐CO
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for the extraction and separation of herbal analytes. In addition, it presents a critical appraisal about the advantages and disadvantages of SFE technique in comparison with traditional extraction methods, that is, Soxhlet, hydrodistillation (HD), and head space extraction. The abilities, advantages, shortcomings, and prospects of SFE for isolation and extraction of volatile components and essential oil of plant materials are also discussed.