In this study, thin‐layer chromatography was applied for selective extraction of volatile compounds in perfume prior to analysis with solid phase microextraction and gas chromatography—mass spectrometry. The standard compounds were desorbed from the thin‐layer chromatography plate and extracted at 80°C for 15 min showing good linearity of the calibration curves (R2 > 0.98) and acceptable recovery range (65–81%). The plate after the separation was cut into four smaller parts followed by solid phase microextraction/gas chromatography—mass spectrometry analysis, which revealed different compound profile in each part with the correlation between log P of the standard compounds and their positions along the thin‐layer chromatography plate (R2 = 0.65). This approach was applied to analyze perfume compounds in the sample with strong matrix interference from the synthetic agarwood. Terpene hydrocarbons (woody‐based odors), ketones/esters, aldehydes, ethers, and alcohols were mostly observed at 8 ± 1, 6 ± 1, 5 ± 2, 4 ± 2, and 3 ± 2 cm, respectively, from the bottom of the thin‐layer chromatography plate. While, the conventional solid phase microextraction/gas chromatography—mass spectrometry analysis of this sample solution revealed only 62 compounds (including 35 perfume compounds), the four‐piece approach resulted in 109 compounds (62 perfume compounds). Furthermore, the capability of thin‐layer chromatography‐Gas Analyzer approach to analyze the isomers in this complex sample was demonstrated.
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