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Exploring Caffeine Extraction Using Hydrophobic Deep Eutectic Solvents: Experimental and Theoretical Approaches.

Khatereh A Pishro1, Leandro S Silva1, Rafaela S Lamarca1

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Hydrophobic deep eutectic solvents (HDESs) offer a sustainable alternative for caffeine extraction from coffee beans and other sources. The dl-menthol/acetic acid HDES demonstrated superior efficiency and greenness compared to traditional solvents.

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Area of Science:

  • Green Chemistry and Sustainable Extraction Technologies
  • Analytical Chemistry and Spectrophotometry
  • Solvent Science and Engineering

Background:

  • Traditional organic solvents pose environmental and health risks in liquid-liquid extraction.
  • Hydrophobic deep eutectic solvents (HDESs) are emerging as eco-friendly alternatives due to their biodegradability and low toxicity.
  • Efficient extraction of bioactive compounds like caffeine is crucial for various industries.

Purpose of the Study:

  • To investigate the efficacy of specific HDESs (dl-menthol with acetic or hexanoic acid) for caffeine extraction.
  • To optimize extraction conditions and evaluate the performance of HDESs against traditional solvents.
  • To assess the sustainability and greenness of the developed HDES-based extraction method.

Main Methods:

  • Solvent screening using COSMO-RS modeling to identify promising HDES systems.
  • Caffeine extraction from coffee beans, coffee skin, and guaraná drink using selected HDESs.
  • Quantification of extracted caffeine via UV/vis spectrophotometry with Gaussian fitting for spectral interference minimization.
  • Determination of optimal extraction parameters (temperature, solvent ratio) and method validation (precision, LOD, LOQ).
  • Evaluation of method sustainability using the Analytical GREEnness (AGREE) metric.

Main Results:

  • The dl-menthol/acetic acid HDES achieved higher caffeine extraction yields (0.765 mg/100 mg from coffee beans) compared to dl-menthol/hexanoic acid (0.610 mg/100 mg).
  • Optimal extraction conditions were found at 65 °C with a 1:1 solution to solvent ratio.
  • The method demonstrated high precision (SD ±0.0826 mg L⁻¹) and low detection/quantification limits (0.674 and 2.04 mg L⁻¹, respectively).
  • The HDES method achieved a high AGREE score of 0.83, significantly outperforming traditional solvents like dichloromethane and chloroform.

Conclusions:

  • HDESs, particularly dl-menthol/acetic acid, are effective and sustainable solvents for caffeine extraction.
  • The developed method aligns with green chemistry principles, offering a safer and more efficient alternative to conventional extraction techniques.
  • Both theoretical modeling (COSMO-RS) and experimental validation support the potential of HDESs in green extraction processes.