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Article

Valorization of Cocoa Bean Shell Agro-Industrial Residues for Producing Functional Hot Water Infusions

by
Elizabeta Hernández-Domínguez
1,
Vicente Espinosa-Solís
2,
Rocio Guadalupe Hernández-Nava
3,
Raquel García-Barrientos
4,
Carmen del Pilar Suárez-Rodríguez
2,
Pável Gallardo-Bernal
3,
Víctor Manuel Figueroa-Wences
3 and
María de la Luz Sánchez-Mundo
5,*
1
Tecnológico Nacional de México/ITS de Acayucan, Costera del Golfo km 216.4, Col. Agrícola Michapan, Acayucan 96100, Veracruz, Mexico
2
Coordinación Académica Región Huasteca Sur, Universidad Autónoma de San Luis Potosí, Km 5, Carretera Tamazunchale-San Martin, Tamazunchale 79960, San Luis Potosí, Mexico
3
Escuela Superior de Nutrición y Ciencia de los Alimentos Campus Llano Largo, Universidad Autónoma de Guerrero, Carretera Cayaco-Puerto Márquez Parcela 56, 57 y 58, Acapulco 39906, Guerrero, Mexico
4
Laboratorio de Procesos Biotecnológicos, Universidad Politécnica de Tlaxcala, Avenida Universidad Politécnica No. 1, Tepeyanco 90180, Tlaxcala, Mexico
5
Tecnológico Nacional de México/ITS de Las Choapas, Carretera Las Choapas-Cerro de Nanchital Km 6.0, Col. J. Mario Rosado, Las Choapas 96980, Veracruz, Mexico
*
Author to whom correspondence should be addressed.
Processes 2024, 12(12), 2905; https://doi.org/10.3390/pr12122905
Submission received: 1 November 2024 / Revised: 11 December 2024 / Accepted: 14 December 2024 / Published: 19 December 2024
(This article belongs to the Special Issue Promising Analytical and Technological Strategies for Agri-Food Waste Valorisation)
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Abstract

Cocoa bean shell (CBS) is one of the main by-products of the cocoa processing industry and represents about 20% of the bean. This product has been suggested as a food ingredient due to its aroma, high dietary fiber, and polyphenol contents. This work shows the effect of grinding degree (GD) and grinding method on the physicochemical characteristics, total phenolic content (TPC), and antioxidant activity of an aqueous infusion of CBS. Three particle sizes of CBS powder and two milling methods (mechanical and electrical) were used to prepare a hot water infusion. The infusions presented a pH in the range of 5.37–5.80. In both husks and independently of the GD and the grinding method, the TPC was higher than 141 mg of gallic acid equivalent per g (GAE/g), an antioxidant activity greater than 304 µg of Trolox equivalent per g (µgTE/g). The results indicate that CBS can be an excellent alternative for the design of biofunctional beverages, giving added value to this agro-industrial residue of southeastern México.

1. Introduction

Cocoa (Theobroma cacao L.) is one of the agro-food products of Neotropical origin with the most excellent acceptance in the international market, and its exports in grain represent more than 71%. Cocoa products originate in the processing chain, during which the cocoa beans are removed from pods, fermented, and dried for storage and transportation. The cocoa pod husk obtained represents 70–80% of the dry matter of the fruit [1], which implies a large area for disposal and a challenge in managing these residues. The biovalorization of agri-food wastes has attracted great interest in recent years because they contain bioactive compounds of interest, which can add value and contribute to the circular economy [2].
This cocoa industry generates large quantities of waste, with records of up to 20 tons for each ton of dry cocoa beans processed [3]. Cocoa bean shell (CBS) is the residue obtained after extracting the cocoa pulp, a low-cost by-product, is one of the most innovative strategies for valorization, and according to the new trends directed towards the bioconversion of a residue from chocolate processing, it is now considered a food ingredient [3]. Every year, more than 700,000 tons of cocoa shells are produced worldwide, leading to an accumulation issue, which represents an environmental problem due to the lack of agro-industrial waste management strategies [4].
With the latest advances in CBS applications, these by-products represent a great source of bioactive and fiber-rich compounds that may be of interest to the food industry. Some of these molecules are phenols (catechin, epicatechin, and procyanidin B2) and carboxylic acids (protocatechinic acid, salicylic acid, citric acid, and tartaric acid), flavonoids (quercetin, quercetin-3-O-glucoside and quercetin-3-O-rhamnoside, procyanidins, anthocyanins, flavonones and flavonol glycosides 1-6, terpenoid-derived metabolites, lignin, pectin, theobromine), and free amino acids (glutamine, asparagine, serine, and lysine), among others [5]. Several authors have reported that these biomolecules present in CBS offer benefits to human health, such as antioxidant activity, the prevention of oxidation of low-density lipoproteins (LDLs), the reduction or blocking of inflammatory substances [6,7], and a lower risk of cardiovascular disease (CVD) [8,9,10], among others.
Other applications of the biofunctionality of the physicochemical contained in CBS are the antimicrobial, antimutagenic, and antitumor properties that have attracted the pharmaceutical industry’s attention [11,12] and other markets [13]. Thus, considering the potential of these bioactive molecules, cocoa by-products can be used as functional ingredients in various products, such as cereal bars [14,15], bakery products in powder form, biscuits [14] as a substitute for wheat flour on some of the chocolate cake [16], and confectionery and the development of new functional milk beverages [16].
Today’s consumers prefer beverages with high nutritional values that can bring health benefits, considering the nutritional claims on the packing before making the purchase [17]. This has, consequently, driven the search for new formulations with these characteristics.
The developed antioxidant-rich beverage may help human health due to beneficial effects, like anti-inflammatory and neuroprotective properties, owing to their ability to counter oxidative stress [18]. The phenolic compounds in liquid matrices are more readily available for absorption. In contrast, those present in solid matrices require extraction through mechanical, chemical, and enzymatic processes to enhance their absorption by the gastrointestinal tract [18].
Similar agro-industrial by-products, such as coffee hulls and pomegranate peels, have shown potential in functional beverage formulations due to their high antioxidant content. CBS, for example, offers additional advantages, such as a unique aromatic profile and increased availability from cocoa processing. This by-product showed high antioxidant activity in the beverage when compared to four commercial brands of green tea, demonstrated good sensory qualities, and showed to be economically viable for use in commercial beverages. For instance, Singh et al. (2024) [18] have utilized pomegranate peel to create a beverage packed with antioxidants using the hot water infusion technique.
Additionally, grinding processes aimed at reducing particle size exhibit a favorable impact on the chemical composition, physicochemical attributes, and techno-functional properties. Therefore, grinding is a traditional technique, and when the plant material is crushed, it increases the surface area of the mixture with the solvent, allowing for a better extraction of the bioactive compounds [19]. This augmentation results in an increased concentration of bioactive compounds and enhanced antioxidant activity in CBS powders, thereby furnishing valuable insights for optimizing beverage production processes [20]. Notably, there is a lack of reported information regarding the employment of grinding and sieving methods in this context.
This indicates that there is a proportional relationship between the extraction method and the chemical compounds present in the beverages obtained from CBS. This study is designed to use sieved powder derived from two different milling methods, Electric and Mechanical Grinding, using cocoa bean shell. Therefore, the objective was to revalorize agro-industrial cocoa shell wastes to produce low-cost functional hot water infusions, evaluating the presence of total phenols and antioxidants.

2. Materials and Methods

2.1. Raw Material

The pre-toasted cocoa bean shell (CBS) was sourced from Grupo Alerlit S.A de C.V, (Estado de México, México) which has the following certifications for its products: women owned, kosher, and Food and Drug Administration (FDA) (Silver, Spring, MD, USA) approved. Therefore, the CBS used in this study is within the standards of food safety requirements. CBS was acquired in May 2024. CBS was stored in hermetically sealed bags and placed in a dry place protected from light.

2.2. Samples

The grinding of the CBS was carried out by Mechanical Grinding (MG) using a manual disc mill (Model MM-E, Estrella®, Nuevo Léon, México) and Electric Grinding (EG) using an electric coffee grinder (Model GT2035MX/6W0-2419, T-Fal®, Rumilly, France). The CBS powders were separated using three different sieves (MONT INOX®, Monterrey, México) with mesh numbers of 40 (250–150 µm), 60 (380–250 µm), and 100 (<150 µm). Table 1 shows the 6 CBS powder samples that are coded as follows.

2.3. Physicochemical Analysis of CBS

2.3.1. Moisture Content

The moisture content was determined using an OHAUS®, MB23, Parsippany, NJ, USA moisture analyzer thermobalance, following the loss-on-drying method. The calculation involved determining the variance between the samples’ initial and final weights [21]. The analysis was performed in triplicate.

2.3.2. pH

The pH of the CBS samples was determined by the potentiometric method using Microprocessor pH Meter equipment pH 211, Hanna Instruments Inc., Woonsocket, RI, USA.

2.3.3. Color

To determine the color of the cocoa husk powder samples, Petri boxes were used, in which 30 g of the samples were homogeneously distributed. Subsequently, a portable colorimeter was used, which was placed a few cm away from the sample to perform the measurement [22]. They were prepared for the infusions using the protocol that uses 1 g of CBS in 50 mL of water at 80 °C with an extraction time of 20 min. They were allowed to cool and were filtered. In transmittance mode, the color analysis was performed using a spectrophotometer (Konica Minolta®, Tokyo, Japan). L*, a*, and b* CIELab parameters were utilized to quantify the color. L* represents the lightness, ranging from 0 (black) to 100 (white), while a* indicates red-purple (positive) and bluish-green (negative) and b* denotes yellow (positive) and blue (negative). The colorimeter was previously calibrated according to the manufacturer’s recommendation using the standard supplied for blank calibration. All determinations were performed in triplicate.

2.4. Microscopic Granulation Study of CBS Powders

A total of 10 g of ground CBS was placed in a glass Petri dish, and the particle size characteristics were observed using a stereomicroscope (Stemi DV4 Brand ZEISS®, Göttingen, Germany). Photographs were taken randomly in various positions of the Petri dish. The images were analyzed with the Image J 1.53 e application (Java image analyzer) to measure the length (mm) of the cocoa husk particles. The process was performed in triplicate for each sample of each particle size.

2.5. Bioactive Compounds of CBS Powders

2.5.1. Total Phenolic Content (TPC)

The bioactive compounds were extracted using the protocol reported [23] with certain modifications. Briefly, 10 mL of a 50% (1:10 w/v) methanol–water solution was added to 1 g of sample and placed for 120 min under orbital agitation at 120 rpm and was then centrifuged at 3000× g for 10 min. The supernatant was used as an extract. The TPC analysis was conducted spectrophotometrically (Spectrophotometer Bio-Rad Smart SpecTM Plus, Petaluma, CA, USA) at 760 nm using the Folin–Ciocalteu method, as described [24], with some modifications. Initially, 100 µL of the extract was mixed with 125 µL of the Folin–Ciocalteu reagent and allowed to react for 6 min. Subsequently, the reaction was neutralized with 1250 µL of 20% sodium carbonate (Na2CO3) solution. The volume of the mixture was then adjusted to 3 mL with distilled water and stored in the dark for 90 min. The results were determined by interpolation using the gallic acid standard curve for reference and expressed as mg Gallic Acid Equivalent per 100 g Fresh Weight (mg GAE/100 g FW).
In the case of infusions, all the beverages were centrifuged on Prism R centrifuge (Labnet International Inc., Edison, NJ, USA) at 3000× g for 10 min and then passed through a 0.45 m cellulose acetate filter before analyses of TPC.

2.5.2. Antioxidant Activity

To determine the antioxidant activity, an ABTS test (2, 2′-azi-no-bis-(3-ethylbenzothiazoline-6-sulfonic acid) was performed based on the method reported [25] with modifications. For this, solutions of 7 mM ABTS and 2.45 mM potassium persulfate (K2S2O8) were prepared with distilled water. Both solutions were mixed to a 1:1 proportion and left to rest for 12 to 16 h in the dark at room temperature. Before analyzing the samples, the prepared solution absorbance was read at 734 nm; when the reading was greater than 0.7, a dilution with ethanol was made to obtain an absorbance of 0.7 ± 0.02. Subsequently, 2800 µL of the ABTS/potassium persulfate mixture was added to 200 µL of the sample. Finally, the absorbance at 734 nm was monitored every 3 min for 30 min or until at least three constant readings were obtained. The percentage of inhibition in both assays was estimated as a percentage of inhibition (%) = [(A0 − AF)/A0)] × 100], where A0 and AF are the initial and final absorbances, respectively [25]. The standard curves for both assays were obtained by extrapolation using Trolox as the reference oxidizing agent, and the antioxidant activity was expressed as micrograms of Trolox Equivalent per g (µg TE/100 g FW).
In the case of infusions, all the beverages were centrifuged on a Prism R centrifuge (Labnet International Inc., New Jersey, USA) at 3000× g for 10 min and then passed through a 0.45 m cellulose acetate filter before analyses of antioxidant activity analysis.

2.6. Preparation of Hot Water CBS Infusions

The infusions were prepared with each CBS sample using 1 g of CBS in 50 mL of water at 80 °C with an extraction time of 20 min. The infusions were centrifuged on a Prism R centrifuge (Labnet International Inc., New Jersey, USA) at 3000× g for 10 min and then passed through a 0.45 m cellulose acetate filter before analysis. Each infusion was performed in triplicate for evaluation and analysis. Table 2 shows the 6 CBS infusions coded as follows.

Characterization of the CBS Infusions

The infusions obtained were characterized physicochemically (pH and color) and functionally (TPC and antioxidant activity).

2.7. Statistical Analysis

The physicochemical characterization of various samples of cocoa shells and infusions was carried out in triplicate, and the results were evaluated by analysis of variance and subsequent comparison of means using Tukey’s test (p ≤ 0.05) with Minitab® 17 software.

3. Results and Discussion

3.1. Physicochemical Characterization and Antioxidant Capacity of CBS Powders

3.1.1. Moisture Content

The results presented in Table 3 show the moisture content of the CBS samples, with values ranging from 3.33% to 6.70%, indicating levels deemed acceptable for both application and subsequent storage. The moisture content of the cocoa shell is less varied in the Electric Grinding than in the Mechanical Grinding; it could be that these small differences in moisture content observed between the samples of the different grindings can be attributed to the increase in grinding time, although there were no significant differences [26]. It is imperative to underscore the significance of controlling moisture levels to mitigate microbial activity.
The observed quality of the raw material, processing, and subsequent storage depends on moisture content. To produce infusion products, adherence to the permissible moisture limit of approximately 12% for cocoa husk is paramount in preventing degradation and the onset of contamination by molds and yeasts, as stipulated [27].
Similar values have been reported by other authors, for instance, Lares et al. (2018) [28], who noted that the cocoa husk powder had an approximate moisture content of 4.76%. Soto et al. (2012) [29] reported a range of 3.45 to 5.07%, and Garay et al. (2020) [30] reported 3.81% humidity in the roasted husk at 140 °C. CBS from each cocoa industry had different moisture contents; the moisture content of fresh CBS was 12.39–16.75% and 6.41–9.23% for roasted CBS. Djali et al. (2023) [31] reported 5.9% moisture content [21]. The moisture content presented by the CBS samples is influenced by diverse factors, such as climatic conditions, cocoa variety (different pod husk thickness), considering that CBS has been reported to be hygroscopic [32,33], and the different phases of the treatment carried out during the post-harvest (fermentation, drying to roasting temperature, time, among others) [12].

3.1.2. Granulometric Analysis

In Figure 1, the particle sizes of cocoa husk milled using two distinct grinders, namely, mechanical and electrical, are depicted. The samples demonstrated particle sizes falling within the recommended range for the optimal extraction of bioactive compounds [34]. Jumpa et al. (2018) [35] have highlighted the significance of particle sizes ranging between 80 and 300 µm in facilitating the diffusivity of bioactive compounds within the infusion filter.
Furthermore, Xiao et al. (2017) [36] contend that the particle size is a critical parameter that governs the dispersion rate, infusion properties, and release of active components. As per the data, the samples were categorized as follows: coarse particles (diameter < 1000 µm), fine particles (diameter < 100 µm), and ultrafine particles (diameter < 10 µm). MG-CBS-40, -60, and -100 and EG-CBS-40 and -60 were classified as fine particles, while EG-CBS-100 was categorized as ultrafine particles (Figure 1 and Figure 2).
Both types of grinding techniques yielded finely ground powders; however, only the powders processed by the electric grinder and subsequently sieved through mesh 100 were categorized as ultrafine (Figure 2C,F).
These findings provide evidence of discernible variances in the employed size reduction methods. Notably, the coarse roller mill utilized for cocoa bean shell grinding yielded intermediate grinding sizes [37]. It is of significance to note that none of the specimens demonstrate a diameter exceeding 1000 µm, thereby enabling the efficient extraction of bioactive compounds of interest (Figure 2).

3.1.3. Color of CBS Powder and Infusions

In Table 4, the L* parameter exhibited statistically significant variances across different particle sizes (PT). Specifically, samples MG-CBS-40, EG-CBS-40, EG-CBS-60, and MG-CBS-60 demonstrated lower luminosity alongside a dark brown coloration. The luminosity of the CBS decreased as the particle size decreased. In contrast, samples EG-CBS-100 and MG-CBS-100 displayed higher luminosity and a light brown color. Murillo-Baca et al. [38] reported higher luminosity (L*) values for Criollo cocoa shell flours and a greater inclination towards darker colors in comparison to the values obtained in our research.
Notably, samples EG-CBS-40 and EG-CBS-60 demonstrated the lowest luminosity value (~17), indicative of powders ranging from brown to reddish, while the sample MG-CBS-100 recorded the highest luminosity value of 43.23. Powders prepared with CBS milled in an electrical grinder demonstrated a lower luminosity compared to manually milled counterparts. With regards to the a* parameter, the results demonstrated a range of values from 11.78 for EG-CBS-40 to 39.61 for EG-CBS-60, signifying the prevalence of a yellow contribution (positive b* value) and a secondary red contribution (positive a* value), thus enabling the analytical delineation of the extract’s color as brown. It has been asserted that color serves as a determinant of quality and plays a significant role in influencing product acceptance or rejection [34].
As documented by Loza de la Cruz and Inga, 2018 [39], following the roasting of the seeds, the husks acquire a crunchy, brown appearance and emit a distinctive chocolate aroma. These findings signify lower chromatic coordinates compared to those observed in cocoa husk extracts, indicating L* 68.78, a* 17.33, and b* 49.99, representing a medium brown hue [40]. Various authors report that grinding time seems to influence cocoa shell color due to the increase in temperature and by Maillard reactions in which the release of brown compounds, particularly melanoidins, occurs [41], and similar results to those found by Ghodki and Goswami, 2016, were observed [42].
Consequently, the analysis of the study values will facilitate the establishment of precise color standards for the production and marketing of cocoa-based products derived from cocoa bean shells.
The color profiles of the infusions are outlined in Table 4. The findings revealed that the extract primarily stemmed from a dominant yellow component (evidenced by a positive b* value) and, to a lesser degree, a red component (denoted by a positive a* value). The amalgamation of these color components, alongside luminosity, facilitated the analytical characterization of the extract’s color as a medium brown. In terms of luminosity, the parameter L* exhibited statistically significant variances across different particle sizes.
The parameter a* suggests a predisposition towards the red color in samples IEG-C-40, IMGC-40, IMGC-60, and IEGC-60, characterized by a deep red coloring. This trend is followed by a decline in the samples IMGC-100 and IEGC-100, indicating discernible color disparities among the samples. The recorded values of the parameter a* align with those documented [38], suggesting a propensity towards a red coloration in cocoa shell flour.
In parameter b*, it was noted that the samples IMGC-40, IEGC-40, IEGC-60, and IMGC-60 exhibited negative values, indicative of a blue coloration. In contrast, the samples IEGC-100 and IMGC-100 displayed a tendency towards a yellow color, with lighter hues observed in samples featuring smaller particle sizes. These outcomes corroborate the findings [38] about the color intensity (b*), reflecting a propensity towards yellow coloration, which is notably less pronounced in coffee shell than in cocoa shell flour [43]. The study samples display a distinct cocoa-colored attribute, characteristic of beverages containing cocoa.
Below are the different colors obtained from the cocoa husk infusions from mechanical and electric grinding mills (Figure 3). The display of these colors may be due to the milling processes and the characteristics of the raw material. In addition, with 100 mesh, where the particles are finer, the tendency of infusions towards darker colors is shown.

3.1.4. pH of CBS Powder and Infusions

The results of the pH of the samples are presented in Table 5. The pH values ranged from 5.04 to 5.47, and no statistically significant differences (p = 0.05) were detected concerning the grinding type or particle size. This different pH obtained from the two types of milling may be because they leach more organic acids [16]. These pH values are due to the presence of organic acids such as oxalic, citric, succinic, tartaric, malic, and acetic acids [18]. The obtained values coincide with those reported by Aldas-Morejón et al. (2023) [44], who found pH intervals of 5.46–4.69 for cocoa husk samples of the Forastero and CCN51 varieties roasted at 140 °C and 120 °C, respectively.
Garay-Vega et al. (2020) [30] reported pH values for the cocoa husk with three distinct roasting temperatures: the treatment roasted at 120 °C had a pH of 4.69, the treatment roasted at 130 °C had a pH of 4.72, and the treatment roasted at 140 °C had a pH value of 4.91. This variability, which causes the increase in pH, may be influenced by temperature due to the volatilization of the predominant acids [45]. Another theory reported [46] states that pH values are related to the genotype and place of origin of grains.
In the analysis of cocoa husk infusions, it was observed that the pH values ranged from 5.37 to 5.51 (Table 5). Notably, the infusion identified as IEGC-40 exhibited the highest pH value, demonstrating statistically significant variance when compared to the remaining samples due to it having fewer acid compounds, such as alkaloids. Noteworthy is the fact that the electric grinding process with a particle size of 40 yielded the highest pH values, whereas infusions prepared with a particle size of 100 evidenced the lowest pH values.
These findings closely align with the pH values of 4.84 to 5.19 previously reported [32] for six distinct cocoa husk beverages. The pH of an infusion can be impacted by the chemical composition of the plant material, specifically due to the presence of organic acids or alkaloids [47].

3.1.5. Total Phenolic Content (TPC) of CBS Powders

Figure 4 presents the total phenolic content (TPC) results expressed as gallic acid equivalents/g sample. EG was the most effective method for extracting the TPC, allowing greater extraction values (122–131 mg GAE/g FW) than those obtained by MG. Electrical grinding may have led to the generation of ultrafine particles, thereby facilitating the extraction of TPCs.
Although the particle size had no effect on the extraction of phenolic compounds in powders, in the samples obtained from the traditional hot water infusion technique (Figure 4), it was fundamental to increase the content of these polyphenols [48]. These results for CBS infusions are similar to those reported [20], in which an increase in the TPC extraction rate was observed with a decreasing particle size.
The TPC values in cocoa husk have shown variability with a range of 6.04–94.95 mg GAE/g FW, depending mainly on the extraction conditions and solvents used [32,49], the geographical origin, the variety, the harvest season [37], and other factors, such as the type and time of fermentation and the processing temperature of the cocoa bean [12,50]. Although the TPC values are relatively low, they are considered relatively crucial because it is an agro-industrial waste.
On the other hand, there are reports where different phenolic compounds and methylxanthines have been identified from roasted cocoa bean shell (CBS), such as Flavan-3-ols, catechin-3-O-glycosides, N-phenyl-propenoyl-L-aminoacids, procyanidin B-type, and procyanidin A-type [51].

3.1.6. Antioxidant Activity of CBS Powders

The results of the antioxidant activity of CBS powders are depicted in Figure 5. The most noteworthy antioxidant activity was attained using the MG method and a particle size of 40 (MG-CBS-40), yielding a value of 233 µgTE/100 g of fresh weight. The reduction in the uptake of free radicals can be ascribed to the degradation of TPC, which was brought about by elevated temperature and increased friction within the EG and demonstrated the highest antioxidant activity in the smallest particles, registering values of 11.55 mgTE/g consequent to grinding, which may have led to a more significant release of phenolic compounds and thereby inferred greater antioxidant activity.
Nevertheless, in this study, the extracted phenolic compounds were fewer in quantity; however, it is feasible that there existed a variance in the chemical composition, thereby signifying a substantial antioxidant capacity.
Several studies report that the antioxidant properties of CBS are due to the presence of bioactive compounds, such as polyphenols, including catechin, epicatechin, isoquercetin theobromine, caffeine, melanoidins, and proanthocyanidins [41].

3.2. Total Phenolic Content and Antioxidant Activity of CBS Infusions

3.2.1. Total Phenolic Content of CBS Infusions

The total phenolic content present in the CBS infusions is shown in Figure 6. It was observed that the values varied among different types of grinding and particle sizes. The recorded values ranged from 141 mg GAE/g FW for the IMGC-40 infusion to 203 mg GAE/g FW for the IMGC-100 infusion. Notably, the particle size of the cocoa husk did not exert an influence on the TPC. Among the infusions, the IMGC-100 treatment exhibited the highest TPC at 203 mg GAE/g FW, surpassing the 169 mg GAE/g FW obtained with the electric grinding IEGC-100 method.
In the comparison of the total phenolic content (TPC) of CBS powders (Figure 4), it was noted that the TPC was lower (27–220 mg GAE/g FW) than the TPC of the CBS infusions (ranging from 150 to 220 mg GAE/g FW). This disparity may be attributed to the enhanced entrainment of these compounds achieved through the process of grinding and extraction utilizing infusion with hot water.
Previous studies have documented TPC values in certain cocoa husk beverages produced using the Capsule technique with a particle size exceeding 4000 µm, yielding a TPC of 126.86 mg GAE/g FW. For beverages prepared using the Moka technique with a particle size of 500–1000 µm, there was a TPC of 1803.83 mg GAE/g FW, whereas in the Napolitano technique with a size of 250–500 µm, there was a TPC of 1500–1550 mg GAE/g FW [32]. Therefore, this study concluded that the Moka and Neapolitan techniques may be the most effective methods for extracting polyphenols in functional beverages from this agro-industrial residue [32].
Overall, the TPCs detected in the current study were lower than those reported [52] in cocoa husk beverages extracted using two extraction techniques (capsule and tea beverages), with reported values ranging from 320 mg GAE/g FW to 600.48 mg GAE/g FW, respectively. The interplay between temperature and diffusibility is a critical factor in the extraction of bioactive compounds. Temperature has the potential to modulate the diffusion rate of compounds within the sample matrix, thereby impacting both the extraction efficiency and the yield of bioactive compounds obtained [53,54].

3.2.2. Antioxidant Activity of CBS Infusions

The infusions of CBS, produced from powders obtained through mechanical grinding, demonstrated the highest antioxidant activity, regardless of particle size (Figure 7). The IMGC-100 sample (CBS with mechanical milling) was the one that showed the highest and most significant differences in TPCs (p = 0.05) and presented the highest values of 315 µgTE in antioxidant activity compared to the other treatments.
Upon comparing the antioxidant activity of the CBS infusions, it was 35% higher than that of CBS powders, which ranged from 30 to 70% lower, and it was evident that the extraction process significantly affected oxidative capacity. It was more effective than the hot water technique method for the higher extraction of these bioactive compounds. Studies about the effects of particle size and extraction methods on CBS functional beverages have elucidated a direct relationship between particle size and antioxidant capacity in cocoa husk beverages prepared via the percolation technique, demonstrating a proportional increase as the particle size decreases [32,52].
Conversely, beverages obtained through the French press method do not exhibit such dependency on particle size, with the highest levels of antioxidant activity observed in conjunction with larger particle sizes [32]. In plant-based filters, the infusion temperature emerges as a key determinant in achieving optimal phenolic compound levels and antioxidant capacity.
The TPC of CBS was higher (5–8 mg GAE per g [54], that those reported in green tea (3.8–4 mg GAE per g [55] and 1.41 mg GAE/mL [56]. Commercial green tea values were 4.90 micromol Trolox equivalents per mL (µmol eqTx/mL) [47], and pomegranate peel hot water infusion values were 155.78 mg GAE/g.
Furthermore, the findings regarding the antioxidant activity identified in this study hold substantial significance. The prevalent practice of grinding cocoa beans and husks using a traditional manual disk mill remains a viable method. It stands as an excellent alternative for producing a beverage with commendable bioactive characteristics from agro-industrial waste, thereby yielding a functional drink.

4. Conclusions

The moisture content of CBS was different due to the quality of the material, as well as the type of milling, time, processing, and storage. It should be noted that CBS is hygroscopic. The pH of CBS also shows a small variation between electric and Mechanical Grinding, possibly due to the leaching of organic compounds. The smaller grinding particle size of <150 µm allowed for obtaining the most functional infusion using the Mechanical Grinding method with 204 mg GAE/g TPC and 312 µg TE/g antioxidant activity. The color is influenced by the type of grinding, time, and Maillard reactions that release brown compounds, including melanoidins. This study illustrates the feasibility of developing infusions using cocoa bean shells, employing two different types of grinding and three variable particle sizes. The functional CBS infusions showed biological activities, such as antioxidant activity, due to phenolic compounds.
Therefore, the plausibility of obtaining bioactive compounds through Mechanical Grinding and the ability to add value to cocoa husk, an agro-industrial by-product, which can be integrated into the formulation of beverages or functional foods with bioactive compounds, aligning with the principles of circular economy and also strengthening the local economy of the southeastern region of the country, are highlighted.

Author Contributions

Conceptualization, M.d.l.L.S.-M. and E.H.-D.; methodology, M.d.l.L.S.-M. and E.H.-D.; investigation, M.d.l.L.S.-M., E.H.-D., R.G.-B. and R.G.H.-N.; resources, M.d.l.L.S.-M., E.H.-D. and R.G.-B.; writing—original draft preparation, M.d.l.L.S.-M., E.H.-D. and R.G.H.-N.; writing—review and editing, M.d.l.L.S.-M., R.G.H.-N., R.G.-B., C.d.P.S.-R., V.E.-S., V.M.F.-W. and E.H.-D.; visualization, M.d.l.L.S.-M., R.G.H.-N., V.E.-S., P.G.-B., C.d.P.S.-R. and E.H.-D.; funding acquisition, M.d.l.L.S.-M. and E.H.-D. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by Tecnológico Nacional de México, grant number 19852.24-PD Scientific Research, Technological Development, and Innovation Projects 2024.

Data Availability Statement

All data generated or analyzed during this study are available upon request.

Acknowledgments

“This work was published thanks to the support of the Consejo Veracruzano de Investigación Científica y Desarrollo Tecnológico”. The authors thank Tecnológico Nacional de México (TecNM) and the Consejo Nacional de Humanidades, Ciencias y Tecnologías (CONAHCYT) from México.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Particle size determination of cocoa bean shell (CBS). EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. According to Tukey’s Multiple Range Test, values with different letters in the bar indicate significant differences (p < 0.05).
Figure 1. Particle size determination of cocoa bean shell (CBS). EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. According to Tukey’s Multiple Range Test, values with different letters in the bar indicate significant differences (p < 0.05).
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Figure 2. Cocoa bean shell (CBS) milling. (A) EG-CBS-40, (B) EG-CBS-60, (C) EG-CBS-100, (D) MG CBS-40, (E) MG CBS-60, and (F) MGCBS-100.
Figure 2. Cocoa bean shell (CBS) milling. (A) EG-CBS-40, (B) EG-CBS-60, (C) EG-CBS-100, (D) MG CBS-40, (E) MG CBS-60, and (F) MGCBS-100.
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Figure 3. The different colors of cocoa bean shell infusions. IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh.
Figure 3. The different colors of cocoa bean shell infusions. IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh.
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Figure 4. Total phenolic content of cocoa bean shell powder. EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
Figure 4. Total phenolic content of cocoa bean shell powder. EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
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Figure 5. Antioxidant activity of cocoa bean shell powder. Results are presented as means ± SD (n = 3) on a fresh weight basis. EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
Figure 5. Antioxidant activity of cocoa bean shell powder. Results are presented as means ± SD (n = 3) on a fresh weight basis. EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
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Figure 6. Total phenolic content of cocoa bean shell infusions. Results are presented as means ± SD (n = 3). IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh. According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
Figure 6. Total phenolic content of cocoa bean shell infusions. Results are presented as means ± SD (n = 3). IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh. According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
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Figure 7. Antioxidant activity of cocoa bean shell infusions. IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
Figure 7. Antioxidant activity of cocoa bean shell infusions. IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same bar indicate significant differences (p < 0.05).
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Table 1. The 6 samples of CBS powders.
Table 1. The 6 samples of CBS powders.
Samples CBS PowdersCoded
Electrical Grinding of CBS at 40 meshEG-CBS-40
Electrical Grinding of CBS at 60 meshEG-CBS-60
Electrical Grinding of CBS at 100 meshEG-CBS-100
Mechanical Grinding of CBS at 40 meshMG-CBS-40
Mechanical Grinding of CBS at 60 meshMG-CBS-60
Mechanical Grinding of CBS at 100 meshMG-CBS-100
Table 2. The 6 CBS infusions.
Table 2. The 6 CBS infusions.
Samples CBS InfusionsCoded
Infusion Electrical Grinding of CBS at 40 meshIEG-CBS-40
Infusion Electrical Grinding of CBS at 60 meshIEG-CBS-60
Infusion Electrical Grinding of CBS at 100 meshIEG-CBS-100
Infusion Mechanical Grinding of CBS at 40 meshIMG-CBS-40
Infusion Mechanical Grinding of CBS at 60 meshIMG-CBS-60
Infusion Mechanical Grinding of CBS at 100 meshIMG-CBS-100
Table 3. Moisture of cocoa bean shell powders.
Table 3. Moisture of cocoa bean shell powders.
SamplesMoisture (%)
EG-CBS-404.00 ± 0.00 bc
EG-CBS-604.66 ± 0.57 ab
EG-CBS-1005.00 ± 0.00 cb
MG-CBS-403.33 ± 0.57 a
MG-CBS-606.70 ± 0.52 d
MG-CBS-1006.70 ± 0.52 d
EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding of CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding of CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding of CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same column indicate significant differences (p < 0.05).
Table 4. Color parameter of cocoa bean shell powders and infusions.
Table 4. Color parameter of cocoa bean shell powders and infusions.
Powders
Samples L* a* b*
EG-CBS-40 17.62 ± 1.35 c 11.78 ± 0.62 bc 34.8 ± 1.01 bc
EG-CBS-60 17.51 ± 1.83 c 39.61 ± 8.02 a 114.53 ± 13.7 a
EG-CBS-100 36.98 ± 3.07 b 15.97 ± 3.8 bc 47.81 ± 16.07 bc
MG-CBS-40 37.96 ± 1.55 ab 20.0 ± 2.03 b 58.02 ± 8.09 b
MG-CBS-60 38.13 ± 0.95 ab 20.2 ± 1.15 b 57.07 ± 5.29 b
MG-CBS-100 43.23 ± 2.79 a 8.40 ± 0.39 c 24.63 ± 0.74 c
Infusions
IEGC-40 17.85 ± 0.04 b 0.90 ± 0.05 ab −0.23 ± 0.03 c
IEGC-60 17.89 ± 0.03 ab 0.92 ± 0.05 a −0.21 ± 0.04 c
IEGC-100 12.37 ± 0.05 c 0.79 ± 0.09 c 0.50 ± 0.16 b
IMGC-40 17.91 ± 0.05 a 0.88 ± 0.04 ab −0.13 ± 0.03 c
IMGC-60 17.88 ± 0.02 ab 0.94 ± 0.05 a −0.24 ± 0.05 c
IMGC-100 11.99 ± 0.05 d 0.82 ± 0.08 bc 0.62 ± 0.07 a
L*: lightness from black (0) to white (100); a*: green, red color (a* > 0 indicates redness, a* < 0 indicates greenness); b*: blue, yellow color (b* > 0 indicates yellowness, b* < 0 indicates blueness). EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same column indicate significant differences (p < 0.05).
Table 5. pH of cocoa bean shell powders and infusions.
Table 5. pH of cocoa bean shell powders and infusions.
PowdersInfusions
Samples pHSamples pH
EG-CBS-40 5.20 ± 0.11 a IEGC-40 5.51 ± 0.01 b
EG-CBS-60 5.04 ± 0.12 a IEGC-60 5.38 ± 0.03 a
EG-CBS-100 5.40 ± 0.02 a IEGC-100 5.43 ± 0.01 ab
MG-CBS-40 5.47 ± 0.42 a IMGC-40 5.37 ± 0.0 a
MG-CBS-60 5.12 ± 0.14 a IMGC-60 5.39 ± 0.0 a
MG-CBS-100 5.34 ± 0.05 a IMMC-100 5.43 ± 0.01 ab
EG-CBS-40 = Electrical Grinding of CBS at 40 mesh; EG-CBS-60 = Electrical Grinding of CBS at 60 mesh; EG-CBS-100 = Electrical Grinding of CBS at 100 mesh; MG-CBS-40 = Mechanical Grinding CBS at 40 mesh; MG-CBS-60 = Mechanical Grinding CBS at 60 mesh; MG-CBS-100 = Mechanical Grinding CBS at 100 mesh. IEGC-40 = Infusion Electrical Grinding of CBS at 40 mesh; IEGC-60 = Infusion Electrical Grinding of CBS at 60 mesh; IEGC-100 = Infusion Electrical Grinding of CBS at 100 mesh; IMGC-40 = Infusion Mechanical Grinding of CBS at 40 mesh; IMGC-60 = Infusion Mechanical Grinding of CBS at 60 mesh; IMGC-100 = Infusion Mechanical Grinding of CBS at 100 mesh. Results are presented as means ± SD (n = 3). According to Tukey’s Multiple Range Test, values with different letters in the same column indicate significant differences (p < 0.05).
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Hernández-Domínguez, E.; Espinosa-Solís, V.; Hernández-Nava, R.G.; García-Barrientos, R.; Suárez-Rodríguez, C.d.P.; Gallardo-Bernal, P.; Figueroa-Wences, V.M.; Sánchez-Mundo, M.d.l.L. Valorization of Cocoa Bean Shell Agro-Industrial Residues for Producing Functional Hot Water Infusions. Processes 2024, 12, 2905. https://doi.org/10.3390/pr12122905

AMA Style

Hernández-Domínguez E, Espinosa-Solís V, Hernández-Nava RG, García-Barrientos R, Suárez-Rodríguez CdP, Gallardo-Bernal P, Figueroa-Wences VM, Sánchez-Mundo MdlL. Valorization of Cocoa Bean Shell Agro-Industrial Residues for Producing Functional Hot Water Infusions. Processes. 2024; 12(12):2905. https://doi.org/10.3390/pr12122905

Chicago/Turabian Style

Hernández-Domínguez, Elizabeta, Vicente Espinosa-Solís, Rocio Guadalupe Hernández-Nava, Raquel García-Barrientos, Carmen del Pilar Suárez-Rodríguez, Pável Gallardo-Bernal, Víctor Manuel Figueroa-Wences, and María de la Luz Sánchez-Mundo. 2024. "Valorization of Cocoa Bean Shell Agro-Industrial Residues for Producing Functional Hot Water Infusions" Processes 12, no. 12: 2905. https://doi.org/10.3390/pr12122905

APA Style

Hernández-Domínguez, E., Espinosa-Solís, V., Hernández-Nava, R. G., García-Barrientos, R., Suárez-Rodríguez, C. d. P., Gallardo-Bernal, P., Figueroa-Wences, V. M., & Sánchez-Mundo, M. d. l. L. (2024). Valorization of Cocoa Bean Shell Agro-Industrial Residues for Producing Functional Hot Water Infusions. Processes, 12(12), 2905. https://doi.org/10.3390/pr12122905

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