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 des...
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MDPI AG
2025-02-01
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| author | Luciana Lordêlo Nascimento Paulo Natan Alves dos Santos Honnara Santos Granja Larissa da Silveira Ferreira João Victor Ferreira Lima Bruna Louise de Moura Pita Allan dos Santos Polidoro Lisiane dos Santos Freitas Elina Bastos Caramão Fabio de Souza Dias Alini Tinoco Fricks |
| author_facet | Luciana Lordêlo Nascimento Paulo Natan Alves dos Santos Honnara Santos Granja Larissa da Silveira Ferreira João Victor Ferreira Lima Bruna Louise de Moura Pita Allan dos Santos Polidoro Lisiane dos Santos Freitas Elina Bastos Caramão Fabio de Souza Dias Alini Tinoco Fricks |
| author_sort | Luciana Lordêlo Nascimento |
| collection | DOAJ |
| description | 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. |
| format | Article |
| id | doaj-art-8ed17e2cb6b44da68bf550763b6399a8 |
| institution | DOAJ |
| issn | 2304-8158 |
| language | English |
| publishDate | 2025-02-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Foods |
| spelling | doaj-art-8ed17e2cb6b44da68bf550763b6399a82025-08-20T02:53:19ZengMDPI AGFoods2304-81582025-02-0114574010.3390/foods14050740Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean ShellsLuciana Lordêlo Nascimento0Paulo Natan Alves dos Santos1Honnara Santos Granja2Larissa da Silveira Ferreira3João Victor Ferreira Lima4Bruna Louise de Moura Pita5Allan dos Santos Polidoro6Lisiane dos Santos Freitas7Elina Bastos Caramão8Fabio de Souza Dias9Alini Tinoco Fricks10Programa de Pós-Graduação em Ciência de Alimentos, Universidade Federal da Bahia, Salvador 40170-115, BA, BrazilRede Nordeste de Biotecnologia, Universidade Federal de Sergipe, São Cristóvão 49107-230, SE, BrazilPrograma de Pós-Graduação em Química, Universidade Federal de Sergipe, São Cristóvão 49107-230, SE, BrazilPrograma de Pós-Graduação em Ciência de Alimentos, Universidade Federal da Bahia, Salvador 40170-115, BA, BrazilPrograma de Pós-Graduação em Ciência de Alimentos, Universidade Federal da Bahia, Salvador 40170-115, BA, BrazilDepartamento de Análises Bromatológicas, Faculdade de Farmácia, Universidade Federal da Bahia, Salvador 40170-115, BA, BrazilDepartment of Chemistry, Pharmaceutical, and Agricultural Sciences, Università degli Studi di Ferrara, 44121 Ferrara, ItalyRede Nordeste de Biotecnologia, Universidade Federal de Sergipe, São Cristóvão 49107-230, SE, BrazilRede Nordeste de Biotecnologia, Universidade Federal de Sergipe, São Cristóvão 49107-230, SE, BrazilPrograma de Pós-Graduação em Química, Universidade Federal da Bahia, Salvador 40170-115, BA, BrazilPrograma de Pós-Graduação em Ciência de Alimentos, Universidade Federal da Bahia, Salvador 40170-115, BA, BrazilThis 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.https://www.mdpi.com/2304-8158/14/5/740energized dispersive guided extraction (EDGE)cocoa waste valorizationmethylxanthinesoptimizationDoehlert matrixgreen chemistry |
| spellingShingle | Luciana Lordêlo Nascimento Paulo Natan Alves dos Santos Honnara Santos Granja Larissa da Silveira Ferreira João Victor Ferreira Lima Bruna Louise de Moura Pita Allan dos Santos Polidoro Lisiane dos Santos Freitas Elina Bastos Caramão Fabio de Souza Dias Alini Tinoco Fricks Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells Foods energized dispersive guided extraction (EDGE) cocoa waste valorization methylxanthines optimization Doehlert matrix green chemistry |
| title | Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells |
| title_full | Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells |
| title_fullStr | Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells |
| title_full_unstemmed | Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells |
| title_short | Mixture Design and Doehlert Matrix for Optimization of Energized Dispersive Guided Extraction (EDGE) of Theobromine and Caffeine from Cocoa Bean Shells |
| title_sort | mixture design and doehlert matrix for optimization of energized dispersive guided extraction edge of theobromine and caffeine from cocoa bean shells |
| topic | energized dispersive guided extraction (EDGE) cocoa waste valorization methylxanthines optimization Doehlert matrix green chemistry |
| url | https://www.mdpi.com/2304-8158/14/5/740 |
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