Ultrasound-assisted headspace solid-phase microextraction (UA-HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been used for analysis of volatile compounds in dry Tagetes minuta L. The highest extraction efficiency was achieved with a 100-lm polydimethylsiloxane (PDMS) fiber. Different experimental conditions, for example, type of fiber coating, sonication time, extraction time and temperature, and desorption time, were investigated. Thirty compounds were identified by use of this UA-HS-SPME-GC-MS method. Comparison of the method with the commonly used hydrodistillation (HD) method showed that the proposed method is simpler, needs much less sample, requires shorter extraction time and lower temperature, has high trapping ability, and extracts more volatile and thermally sensitive compounds. The major components identified by use of the method were E-ocimenone (10.3%), cis-b-ocimene (4.8%), a-terpinolene (8.4%), trans-caryophyllene (19.7%), germacrene-D (10.0%), and camphor (3.6%).

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