Thin layer chromatography based extraction approaches for improved analysis of volatile compounds with gas...

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.