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...

Full description

Saved in:
Bibliographic Details
Main Authors: 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
Format: Article
Language:English
Published: MDPI AG 2025-02-01
Series:Foods
Subjects:
Online Access:https://www.mdpi.com/2304-8158/14/5/740
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary: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.
ISSN:2304-8158