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Ultrasound-assisted headspace solid-phase microextraction (UA-HS-SPME) and hydrodistillation (HD) methods, coupled to gas chromatography-mass spectrometry (GC-MS), were used for the extraction and analysis of volatile compounds from Hypericum perforatum and Hypericum scabrum collected from two different sites in Iran. In the UA-HS-SPME method, various experimental parameters such as the type of fiber coating, sonication time, extraction time, extraction temperature and desorption time were investigated. The highest extraction efficiency was achieved by a 100-µm polydimethylsiloxane (PDMS) fiber. Consequently, 36 compounds were identified in H. perforatum and H. scabrum samples, using the UA-HS-SPME-GC-MS method, of which 14 were the same in both species. On the other hand, 57 compounds of these species were identified by the HD-GC-MS method, of which 21 were the same. The predominant constituents identified using the UA-HS-SPME method in H. perforatum included β-caryophyllene, α-pinene, γ-cadinene, α-selinene, germacrene-D, limonene and myrcene, and in H. scabrum were α-pinene, nonane, β-pinene and limonene. The common constituents identified by the HD-GC-MS method for H. perforatum involved germacrene-D, limonene, β-caryophyllene, α-pinene, β-pinene and germacrene-B, and for H. scabrum were α-pinene, β-pinene, germacrene-D, nonane, limonene and γ-cadinene. The results about the main constituents of the examined species correspond to the findings of other researchers. Additionally, comparing UA-HS-SPME-GC-MS and HD-GC-MS methods showed that the UA-HS-SPME-GC-MS method is much faster and simpler, and it requires much less sample size and lower temperature.

A low-cost and simple cooling-assisted headspace liquid-phase microextraction device for the extraction and determination of 2,6,6-trimethyl-1,3 cyclohexadiene-1-carboxaldehyde (safranal) in Saffron samples, using volatile organic solvents, was fabricated and evaluated. The main part of the cooling-assisted headspace liquid-phase microextraction system was a cooling capsule, with a Teflon microcup to hold the extracting organic solvent, which is able to directly cool down the extraction phase while the sample matrix is simultaneously heated. Different experimental factors such as type of organic extraction solvent, sample temperature, extraction solvent temperature, and extraction time were optimized. The optimal conditions were obtained as: extraction solvent, methanol (10 μL); extraction temperature, 60°C; extraction solvent temperature, 0°C; and extraction time, 20 min. Good linearity of the calibration curve (R(2) = 0.995) was obtained in the concentration range of 0.01-50.0 μg/mL. The limit of detection was 0.001 μg/mL. The relative standard deviation for 1.0 μg/mL of safranal was 10.7% (n = 6). The proposed cooling-assisted headspace liquid-phase microextraction device was coupled (off-line) to high-performance liquid chromatography and used for the determination of safranal in Saffron samples. Reasonable agreement was observed between the results of the cooling-assisted headspace liquid-phase microextraction high-performance liquid chromatography method and those obtained by a validated ultrasound-assisted solvent extraction procedure.