Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells
This work describes the development of a method for the extraction of methylxanthines from cocoa bean shell (CBS) by employing the novel Energized Dispersive Guided Extraction (EDGE) system. The mixtures were composed of ethanol-methanol-water and the ratio was optimized using a simplex-centroid design. Doehlert design (DD) was used to optimize the variables of temperature and time while using methylxanthine content obtained by HPLC-DAD as an analytical response. The optimized mixture consisted of water-ethanol in a 3:2 ratio. The optimum operating conditions for extraction were achieved at a temperature of 148.5 °C and 382 s. Under optimal conditions, 20.14 mg g<sup>-1</sup> DM of theobromine and 3.53 mg g<sup>-1</sup> DM of caffeine were found in the CBS extract. Methylxanthines were quantified with good linearity, LOQs, LODs, precision, and accuracy. The EDGE system, a newly automated extraction instrument, has proven to be very efficient for the recovery of theobromine and caffeine, and is considered a green extraction procedure, as demonstrated by the analytical greenness metric for sample preparation.
Authors
- Fábio de S. Dias (ORCID: https://orcid.org/0000-0003-2279-0691)
- José L. F. C. Lima (ORCID: https://orcid.org/0000-0002-8906-9826)
- Honnara S. Granja (ORCID: https://orcid.org/0000-0002-4005-1051)
- Luciana Lordêlo Nascimento (ORCID: https://orcid.org/0000-0001-6328-8433)
- Elina Bastos Caramão (ORCID: https://orcid.org/0000-0002-7045-5874)
- Paulo Natan Alves dos Santos
- Lisiane dos Santos Freitas (ORCID: https://orcid.org/0000-0002-6720-8338)
- Alini Tinoco Fricks (ORCID: https://orcid.org/0000-0001-9888-952X)
- Allan dos Santos Polidoro (ORCID: https://orcid.org/0000-0002-4981-908X)
- Bruna Louise de Moura Pita (ORCID: https://orcid.org/0009-0004-3647-0597)
- Larissa da Silveira Ferreira
Institutions
- Universidade Federal da Bahia (BR)
- Universidade Federal de Sergipe (BR)
- University of Ferrara (IT)
- Instituto Nacional de Ciência e Tecnologia de Doenças Tropicais (BR)
Publication Details
- Journal
- Foods
- Published
- 2025-02-21
- DOI
- https://doi.org/10.3390/foods14050740
- Citations
- 8
- Primary Topic
- Food Chemistry and Fat Analysis
- Type
- article
- Field-Weighted Citation Impact
- 9.30
Funders
- Coordenação de Aperfeiçoamento de Pessoal de Nível Superior
- Conselho Nacional de Desenvolvimento Científico e Tecnológico