The
growing demand for high added-value products, such as vanilla-derived
compounds, and increasing environmental regulations make evident the
need to find new sustainable solvents for extraction processes, which
meet both legislative requirements and expected yields. Vanilla-derived
compounds are known for their antioxidant and beneficial properties
for human health. These compounds can be recovered from effluent streams,
promoting decontamination and revaluation of wastewater. The potential
of using neoteric solvents, i.e., biobased solvents and hydrophobic
eutectic solvents, as an alternative to conventional volatile organic
solvents, such as ethyl acetate, for sustainable recovery of vanilla-derived
compounds through liquid–liquid extraction from aqueous environments
was investigated. Three biobased solvents (2-methyltetrahydrofuran,
cyclopentyl methyl ether, and d-limonene) and three hydrophobic
eutectic solvents constituted by menthol and organic acids (1:1 dl-menthol:octanoic acid, 1:1 dl-menthol:decanoic acid,
and 2:1 dl-menthol:dodecanoic acid) were evaluated. The extraction
process was optimized in terms of the stirring time and solvent:feed
volume ratio. The effect of the initial solute concentration was also
analyzed. The extraction efficiency of solvents was determined by
UV–visible spectrophotometry and high-performance liquid chromatography
with diode-array detection. The experimental results indicated that
2-methyltetrahydrofuran yielded the highest extraction efficiency
from a vanilla bean extract solution for both vanillin (95.37%) and
vanillic acid (91.96%) with good repeatability (RSD < 0.40%). Regarding
the rest of the neoteric solvents, cyclopentyl methyl ether and hydrophobic
eutectic solvents provided extraction values between 31.6 and 95.4%
for both vanilla-derived compounds, while d-limonene was
significantly less effective. Finally, a solvent recycling and reuse
study was successfully carried out, showing that 2-methyltetrahydrofuran
stands out as a promising biobased extraction solvent for sustainable
recovery of valuable vanilla constituents.