Vanilla is currently sold as an ethyl alcoholic extract, typically at a concentration of 35% (v/v). Alcoholic extracts have some disadvantages, such as high concentrations of organic residues, long extraction times and the requirement of large volumes when used as a flavoring. In contrast, supercritical fluid extraction (SFE) allows isolation of high-purity oleoresins without co-extraction of undesired organic residues, thereby preserving the desired volatile compounds in vanilla. In this study, we identified and quantified volatile compounds and fatty acids in four oleoresins and two ethanolic extracts of cured Vanilla planifolia Andrews beans following 10 or 20 sun-drying and sweating cycles (SS). SFE was carried out at a pressure of 20 MPa at 40°C, 50°C, or 60°C, and the resulting vanilla oleoresins were analyzed with GC-MS and GC-FID. The major compounds identified in the extracts were o-guaiacol, p-creosol, p-vinylguaiacol, p-hydroxybenzaldehyde, vanillic acid and vanillin.
Experimental solubility data of binary and ternary systems containing vanillin and vanillic acid in supercritical carbon dioxide were carried out in equipment based on the static-synthetic method. Compositions of dissolved solids were determined online via high-performance liquid chromatography with a diode array detector. The carbon dioxide + vanillin, carbon dioxide + vanillic acid, and carbon dioxide + vanillin + vanillic acid systems were studied at (315.00, 324.90, and 334.71) K, (314.91, 324.91, and 334.71) K, and (314.13, 323.67, and 333.17) K, respectively. For all systems the measurements were carried out at pressure range between 8.00 and 30.00 MPa. For binary systems the maximum solubilities were 5.215 × 10 −3 and 2.911 × 10 −5 in mole fraction for vanillin and vanillic acid, respectively. For ternary systems the maximum solubilities were 4.669 × 10 −3 and 2.213 × 10 −5 for vanillin and vanillic acid, respectively. The expanded uncertainties (k = 2) for the measured properties are estimated to be U(P) = 0.04 MPa, U(T) = 0.04 K, and U r (y) = 0.0286 mole fraction. Meńdez-Santiago and Teja, Bartle et al., Kumar and Johnston, and Chrastil models were used to correlate the experimental data. The results from the correlation confirmed the consistency of the reported data.
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