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Article

The Role of Different Roasting Temperatures on the Physico-Chemical Properties, Phenolic Compounds, Fatty Acid and Mineral Contents of Carob (Ceratonia siliqua L.) Fruit Powder

by
Isam A. Mohamed Ahmed
1,
Fahad Y. AlJuhaimi
1,
Mehmet Musa Özcan
2,*,
Nurhan Uslu
2 and
Emad Karrar
3
1
Department of Food Science & Nutrition, College of Food and Agricultural Sciences, King Saud University, Riyadh 11451, Saudi Arabia
2
Department of Food Engineering, Faculty of Agriculture, Selcuk University, 42031 Konya, Turkey
3
Department of Plant Sciences, North Dakota State University, Fargo, ND 58108, USA
*
Author to whom correspondence should be addressed.
Processes 2024, 12(9), 1990; https://doi.org/10.3390/pr12091990
Submission received: 26 August 2024 / Revised: 12 September 2024 / Accepted: 14 September 2024 / Published: 15 September 2024
(This article belongs to the Section Food Process Engineering)
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Abstract

:
In this study, the role of different roasting temperatures on oil amount, total phenolic contents, total flavonoid quantities, antioxidant capacity, polyphenol, fatty acid and mineral profiles of roasted-carob fruit powders was revealed. The oil and protein amounts of the carob powders were specified to be between 0.40 (90 °C) and 0.85% (control) to 8.40 (120 °C) and 10.27% (control), respectively. Total phenolic and flavonoid quantities of the raw (control—unroasted) and roasted carob powders were defined to be between 781.16 (control) and 903.07 mg GAE/100 g (150 °C) to 663.81 (control) and 1141.90 mg/100 g (150 °C), respectively. In addition, antioxidant activities of the carob powders were measured to be between 9.27 (150 °C) and 10.30 mmoL/kg (control). Gallic acid and 3,4-dihydroxybenzoic acid amounts of the carob powders were specified to be between 45.16 (control) and 120.66 (150 °C) to 7.06 (control) and 20.46 mg/100 g (150 °C), respectively. Palmitic, oleic and linoleic acids were the key fatty acids of carob oils. It is thought that the fatty acid compositions of carob powder oil, which is generally subjected to heat treatment, are negatively affected by high temperatures. Especially, the linoleic and linolenic acid amounts of the oil samples decreased significantly after 90 °C. The highest element was potassium, followed by Ca, P, Mg, S, Fe, Na, Pb, Cu, Zn B and Mn, in descending order.

1. Introduction

Evergreen (Ceratonia siliqua L.) is a perennial legume plant that has grown in the Mediterranean region since ancient times [1,2,3]. The pulp, which constitutes 90% of the carob fruit, has high sugar and tannin content and low protein and fat content [4,5]. In Turkey, carob is also consumed as fruit, molasses, or made into carob flour. Carob molasses is a preferred product, due to its nutritional properties and high energy value. Since this product does not contain theobromine and caffeine and also contains high amounts of sugar, it is widely used as a cocoa substitute in the food industry [6]. After the slightly sweet carob fruit is dried and turned into powder, carob flour is used in cakes, cookies and chocolates, and in the production of chips or syrup. Crushed broad beans, which can be used to make beverages, are also used in the production of compotes, liqueurs and syrups in Turkey, Malta, Portugal, Spain and Sicily [5,7]. Carob powder, obtained by removing the seeds from the ripe carob fruit and grinding the remaining part, is an alternative food ingredient that can often be used instead of cocoa, because it does not contain caffeine and theobromine [8].
Recently, major polyphenols in carob fibers have been isolated and identified. In addition, the differences and compositions of phenolic compounds in carob bark were investigated. Variety of origin, location and harvest time have been reported to be effective for the chemical composition of carob parts [9]. There are also studies on improving or enriching the properties of various foods by using carob flour or molasses [10]. Roasting processes and conditions have been reported to cause significant physico-chemical changes in the color, aroma, fatty acid profile, phytochemicals and bioactive compounds of vegetable oils (edible seeds and nuts). Roasting treatment disrupts the integrity of the cellular components and causes destroying of the covalent bonds between the phenolic compounds and cell wall, thereby promoting the release of bound phenolic and flavonoid compounds [11].
Products such as milk to be used in the production of pasta, tarhana and yoghurt were enriched with carob flour, and the quality criteria of these products were examined. The number of antioxidants increased in the final product, and there was no negative change in sensory quality criteria [6,10]. At the same time, carob fruit powders were often used instead of cocoa in chocolate production. Recently, many polyphenols such as gallic acid and catechin have been isolated and identified in carob fibers [7].
Several studies have been conducted on the biological activity of carob barks as antidiarrheal agents. Carob fruit fiber has the ability to modulate blood lipid profile in humans. Carob fruits are used primarily in confectionery, beverages, bread or traditional foods such as pasta and kuki in several countries in the Mediterranean region [12,13]. The carob fruits are rich in calcium, phosphorus and potassium, and are an alternative mineral source [12]. The novelty of these studies is that carob powder is a natural product that can be used as a cocoa substitute in both nutritious and bakery products. In addition to bakery products, carob flour is used for other preparations such as pasta, or snacks, milk desserts, solid foods such as cakes, cookies and biscuits, baby foods, drinks, and even breads [7].
It is known that exposure of plant materials to high temperatures has a negative effect on phenolic compounds. Here, the change of different temperatures on the phenolic component amounts on carob fruit flour will be determined. The purpose of this investigation was to reveal the role of different roasting temperatures on oil amount, total phenolic contents, total flavonoid quantities, antioxidant capacity, polyphenol, fatty acid and mineral profiles of roasted-carob fruit powders.

2. Material and Methods

2.1. Material

After the carob fruits were provided from Mersin (Silifke) province (36–37° north latitudes and 33–35° east longitudes), they were transferred to the laboratory in paper bags. The fruits were separated from the stems and seeds and washed with distilled water and dried immediately by laying on a clean surface. Carob fruits were air dried and then ground into powder in a mill. After the carobs dried in air were crushed into large pieces, they were ground in the mill (Arzum AR1034 Clipper coffee grinder (stainless steel, 150 W motor power, 50 g capacity)) and turned into powder (10 mesh). Then, the carob powder was roasted in an oven at three different temperatures (90, 120 and 150 °C) for 15 min.

2.2. Methods

2.2.1. Moisture Content

The KERN & SOHN GmbH infrared moisture analyzer was used for the moisture analysis of the carob powders.

2.2.2. Protein Content

Protein amount of the carob powders was assessed according to the AOAC [14] method.

2.2.3. Color Measurements

A Minolta Chroma Meter CR-200 (Minolta Camera Co. Ltd., Osaka, Japan) was used for measurement of L*, a*, b* values of raw and roasted carob-fruit powders. C.I.E. system—L* a* b* (CIELAB). L*: defines the difference between light (L* = 100) and dark (L* = 0). a*: defines the difference between green (−a*) and red (+a*). b*: defines the difference between blue (−b*) and yellow (+b*). Calibration was carried out with the white color calibration tile before the measurements.

2.2.4. Oil Content

The oil was extracted from carob powder with petroleum ether (Merck, Darmstadt, Germany) by the Soxhlet Apparatus at 50 °C for 6 h, and then the petroleum ether in the micelle was removed with a vacuum evaporator at 50 °C. Then, the oil contents of the samples were determined (%) [14].

2.2.5. Extraction Procedure

Extraction of the carob samples was carried out according to the method recommended by Durazzo et al. [15]. After powdered samples (3 g) were mixed with 20 mL of acidic methanol ((Merck, Darmstadt, Germany): water (80:20 v/v, pH 2), the solution was stored in a rinsing bath for 1 h, followed by centrifugation (Hermle Z-200A, Germany) at 2817 g for 10 min. The supernatants collected in this process, which was performed twice, were filtered.

2.2.6. Total Phenolic Content

The Folin–Ciocalteu (Sigma) chemical was used to assess total phenolic quantities of the carob extracts, and this was established according to the report suggested by Yoo et al. [16]. After preprocessing, the absorbance was read at 750 nm. The findings are defined as mg gallic acid equivalent (GAE)/100 g (dw).

2.2.7. Total Flavonoid Amount

The total flavonoid amount of the carob fruit powder was established according to the study suggested by Hogan et al. [17]. A total of 0.3 mL of NaNO2 (Merck, Darmstadt, Germany), 0.3 mL of AlCl3 (Merck, Darmstadt, Germany) and 2 mL of NaOH (Merck, Darmstadt, Germany) solutions were used for this analysis, and after these chemicals were added to the extract, it was stored in the dark for 15 min. The absorbance was assigned at 510 nm. The findings are described as mg quercetin (QE)/100 g (dw).

2.2.8. Antioxidant Capacity

1.1-diphenyl-2-picrylhydrazyl (DPPH) (Sigma) was used to assess the antioxidant capacity of the carob extracts [18]. After preprocessing, the absorbance was read at 517 nm. The findings are defined as mmol trolox (TE)/kg (dw).

2.2.9. Determination of Phenolic Profiles

Chromatographic separation of the phenolic profiles of the carob powders was conducted by HPLC (Shimadzu LC 10A vp, Kyoto, Japan) montaged with a PDA detector and an Inertsil ODS-3 (5 µm × 4.6 × 250 mm) column. The peaks were taken at 280 using a PDA detector. The mobile phase was a mixture of 0.05% acetic acid in water (A) and acetonitrile (B), with the flow rate of 1 mL/min at 30 °C. It was a linear gradient in this stage. In the analysis of phenolic compounds, the identification and amounts of phenolic compounds were determined by using external standards for each compound.

2.2.10. Fatty Acid Composition

Gas chromatography (Shimadzu GC-2010) montaged with a flame ionization detector and capillary column to determine fatty acid methyl esters of carob oil esterified according to the method ISO 5509 [19] was used. Mobile phase was nitrogen with 1.51 mL/min flow rate. Column temperature was programmed 120 °C for 5 min and increased 240 °C at 4 °C/min and held 25 min at 240 °C. In the analysis of fatty acids, the identification and amounts of fatty acids were assigned by using external standards for each compound.

2.2.11. Determination of Mineral

After weighing 0.5 g of powdered carob fruit, the sample was burned in a microwave system (Cem-MARS Xpress) using 5 mL 65% HNO3 (Merck, Darmstadt, Germany) and 2 mL 35% H2O2 (Merck, Darmstadt, Germany). The volumes of the samples were completed to 20 mL with ultra-deionized water, and the mineral amounts of the samples were analyzed with ICP-AES (Agillent, 5110; Germany).
Working conditions of ICP-AES:
Instrument: ICP-AES (Agillent, 5110; Germany).
RF Power: 0.7–1.5 kw (1.2–1.3 kw for Axial).
Plasma gas flow rate (Ar): 10.5–15 L/min. (radial) 15 “ (Axial).
Auxiliary gas flow rate (Ar): 1.5 “.
Viewing height: 5–12 mm.

2.3. Statistical Analyses

The averages of the analyzes performed three times were taken, and the data were subjected to variance analysis. Significant changes between control results and roasting temperatures were assessed by Duncan’s Multiple Range Test (DMRT) (p < 0.05).

3. Results and Discussion

3.1. Physical and Bioactive Properties of Raw (Control) and Roasted Carob Powder

The chemical properties (oil, total phenolic and flavonoid values and antioxidant activity) of raw (control) and roasted carob powder are depicted in Table 1. The moisture quantities of the raw and roasted carob powder were assessed to be between 3.34 (150 °C) and 8.84% (control), while the oil amounts of the carob powder samples are defined as being between 0.40 (90 °C) and 0.85% (control). Crude protein quantities of raw and roasted carob powders were specified to be between 8.40 (120 °C) and 10.27% (control). The protein quantity of the carob powder decreased with the heat treatment. The reason for this decrease is probably due to the denaturing of the protein with temperature.
Total phenolic and flavonoid amounts of raw carob powder and carob powders roasted at different temperatures were established between 781.16 (control) and 903.07 mg GAE/100 g (150 °C) to 663.81 (control) and 1141.90 mg/100 g (150 °C), respectively. In addition, antioxidant capacities of the carob powders varied between 9.27 (150 °C) and 10.30 mmoL/kg (control). The differences between total phenol, total flavonoid contents and antioxidant activity values of raw and roasted carob flour were found to be statistically significant (p < 0.05). As seen in Table 1, L*, a* and b* results of the carob powder samples are displayed in Table 1. L* values of the carobs were equal to 45.08–61.57. The brightness of samples (L* values) showed a decrease after heat treatment, and the lowest L* value was monitored in the sample roasted at 150 °C. Similar to the results of L* value, roasting temperature had a significant effect on both a* and b* values. a* values of carob samples varied between 4.05 and 11.23, while b* values of samples ranged from 24.59 to 28.66. The roasting process caused an increase from 4.05 to 11.23 in a* values of samples. The highest redness (11.23, a* value) was determined in the sample roasted at 150 °C. However, a reduction from 28.66 to 24.59 was obtained in b* values (yellowness) with the roasting process. Depending on the roasting temperatures, the oil content, L*, a*, b* values, and total phenol contents of carob powders were found to be statistically significant (p < 0.05). In addition, no difference was found between the antioxidant values of the control and 90 °C roasted carob powders. In addition, the protein contents of the carob powders roasted at 120 and 150 °C were found to be statistically similar.
The color values L*, a*, and b* of carob powders were recorded as 41.58–52.55, 10.57–13.49, and 16.63–22.06, respectively [20]. Additionally, there was a decrease in L* and b* values; an increase in the values was detected with increasing roasting time [20]. A similar reduction in L* (from 68.71 to 48.13) and b* (from 22.33 to 11.33) values, and an increase in a* (from 8.61 to 17.99) value of the carob powder were revealed by Eldeep and Mosilhey [21]. The changes in L*, a*, and b* values are related to the Maillard reaction and caramelization [22]. Both the moisture and oil quantities decreased, together with the roasting temperature increase. Also, while the total phenolic and flavonoid quantities of roasted carob powders, compared to control, increased, the antioxidant activity values of roasted carob powders decreased. The possible reason for the increase in the total phenol and flavonoid quantities with the roasting temperature may be due to the Maillard reaction products, with heat. It is thought that the total phenolic content of the samples increased due to the combination of Maillard reaction products and Folin–Ciocalteu [22]. Accordingly, the decrease in antioxidant activity values of carob powders may probably be due to the damage of phenolic components as a result of the applied heat treatment. The carob flour contains 5.9% protein, 0.5% lipid, 8.1 mg GAE/g (dw) total phenol and 8.1 mg QE/g (dw) flavonoid [23]. The carob powder contains low levels of fat (1.99%) and protein (6.34%) [8]. Carob fruit contains 1–5% protein and 0.2–0.8% lipid [12,24]. Kumazawa et al. [25] assessed 19.2 g GAE/100 g total phenol in the carob pod. The quantity of total phenolics changes steadily with an increase in the time of roasting. Petkova et al. [23] determined the antioxidant capacity of carob flour as 70.4 mM TE/g ka (DPPH test) and 84.2 mM TE/g ka (FRAP test). In addition, roasting activates the Maillard reaction, and it has been reported that some of the resulting Maillard reaction products react with the Folin–Ciocalteu chemical and show antioxidant properties [26]. It has been reported that increased release of phytochemicals such as phenolic acids may also cause an increase in total phenol content [27]. In a previous study, the Maillard reaction products formed in peanuts after thermal processing increased the antioxidant capacity of peanuts [28]. Roasted soybeans were established to have significantly higher antioxidant activity than unroasted soybeans. This may be due to an increase in phenolic acids, possibly due to the increased release of phenolic acid phytochemicals from cell matrices [29,30]. The difference between the results obtained in this study and the literature values (120–180 °C (usually about 150 °C) for 10–60 min) [31] may be due to the different roasting temperatures applied. It has been reported that thermal treatments such as roasting can result in the degradation of insoluble phenolic compounds and concentration of antioxidants that can be better extracted [29].

3.2. The Phenolic Compounds of Raw and Roasted Carob Powders

The phenolic constituent quantities of raw and roasted carob powders are defined in Table 2. Gallic acid, 3,4-dihydroxybenzoic acid, catechin, rutin and ferulic acid were established to be at the highest quantities in raw and roasted carob powders (Figure 1). While gallic acid values of the carob powders were assigned to be between 45.16 (control) and 120.66 mg/100 g (150 °C), 3,4-dihydroxybenzoic acid values of the carob powders were assigned to be between 7.06 (control) and 20.46 mg/100 g (150 °C). Catechin and caffeic acid quantities of the raw and roasted carob powders were characterized to be between 13.65 (control) and 68.86 (150 °C) to 2.56 (control) and 18.67 mg/100 g (120 °C), respectively. Syringic acid and rutin quantities of the carob powder samples were specified to be between 1.95 (90 °C) and 33.47 (120 °C) to 16.79 (control) and 39.63 mg/100 g (150 °C), respectively. While p-coumaric acid quantities of the carob powders vary between 2.58 (control) and 8.99 mg/100 g (150 °C), ferulic acid quantities of the raw and roasted carob powders were identified to be between 4.19 (90 °C) and 10.25 mg/100 g (150 °C). Resveratrol and quercetin quantities of raw and roasted carob powders were found to be between 0.35 (control) and 2.63 mg/100 g (90 °C) to 0.83 (control) and 6.27 mg/100 g (120 °C), respectively. Since quercetin is a flavonoid, it has an antioxidant effect. However, since resveratrol is a non-flavonoid polyphenol belonging to the stilbenoid group, its antioxidant effect may be quite low. Also, cinnamic acid values of the carob powders were established to be between 1.29 (150 °C) and 2.32 mg/100 g (120 °C). Kaempferol quantities of raw and roasted carob powder samples were established to be under <0.54 mg/100 g (120 °C). It was observed that there were statistically significant differences among phenolic constituent amounts of raw (unroasted) carob powder and carob powder roasted at different temperatures (p < 0.05).
Carob fruits contains lots of polyphenols, especially highly condensed tannins, gallic acid, (+)-catechin and quercetin glycosides [12,32,33]. The gallic acid quantity of carob fruit is estimated to be between 23.7 and 164.7 mg/100 g [7,12,34]. Ayaz et al. [12] assessed 1249.5 gallic acid, 3.6 syringic acid and 1.8 µg/g sinapic acid in carob fruits. The gallic acid, pyrogallol, protocatechuic acid, chlorogenic acid, catechin, catechol, and cinnamic acid amounts of the carob flour were assessed as 10.21, 4970.18, 71.47, 101.09, 27.97, 164.67, and 7.78 [8].
The phenolic profile quantities of the carob powders roasted at different temperatures increased significantly, according to the control. In general, the most observed increase in the amount of phenolic profiles was observed in carob powder roasted at 150 °C. The quantities of some phenolic constituents showed changes depending on the increase in temperature. Generally, the phenolic compound amounts of carob powder roasted at 150 °C increased approximately 2 to 2.5 times compared to the control. In addition, cinnamic acid content increased at 90 and 120 °C, compared to the control, and partially decreased at 150 °C. Generally, the phenolic quantities of the carob powders roasted at 150 °C were higher than that of control. The contents of gallic acid, 3,4-dihydroxybenzoic acid, 1,2-dihydroxybenzene, p-coumaric acid, resveratrol, kaempferol, and naringenin of coffee bean roasted in a traditional oven were established to be at a high level, compared to the microwave. But, in general, the amounts of phenolic components of coffee roasted in both microwave and oven were found to be high, compared to the control group [27]. In general, our phenolic results showed similarity with the previous study results [27].
Depending on the temperature and time, it can be said that the differences in phenolic profile quantities of carob powder dried at different temperatures were compared with the control group. These changes are probably due to ground form, particle sizes, variety, and roasting and extraction conditions.

3.3. The Fatty Acid Composition and Amounts of the Raw and Roasted Carob-Powder Oils

The fatty acid profile and quantities of the raw and roasted carob-powder oils at different temperatures are displayed in Table 3. While palmitic acid values of the carob powder oils vary between 10.02% (control) and 16.19% (90 °C), stearic acid values of carob powder oils were established to be between 5.19% (90 °C) and 8.41% (120 °C) (Figure 2). Also, oleic and linoleic acid amounts of the carob powder oils roasted at different temperatures were stated to be between 29.55 (control) and 36.27 (90 °C) to 17.30 (control) and 36.99% (90 °C), respectively. Linolenic acid amounts of the carob powder oils were defined to be between 22.39 (120 °C) and 46.17% (90 °C). The amounts of arachidic and behenic acids in raw and roasted carob-powder oils were detected to be below <0.75%. The applied roasting temperatures had an effect on the fatty acid content of the oils extracted from the carob powders, and the fatty acid compositions of the oils of the carob powders roasted at each temperature were found to be statistically significant (p < 0.05). The highest quantities of saturated fatty acids were established in carob powder oil roasted at 90 °C. In general, the quantities of fatty acids in roasted carob powder oils at different temperatures compared to the control have increased. However, the palmitic acid quantity of carob powder oil roasted only at 120 °C was higher than the palmitic acid value of carob powder oil roasted at both control and 90 and 120 °C. The fatty acid profile of the carob powder oil, which is generally subjected to heat treatment in atmosphere conditions, is adversely affected by high temperature. The linoleic and linolenic acid amounts of the oil samples, especially, decreased significantly after 90 °C. These reductions were seen more in unsaturated fatty acids. Moreover, no significant decrease was observed in palmitic and stearic fatty acids. On the contrary, palmitic acid values of roasted carob powder oil were found to be slightly increased when compared to the control. Changes in fatty acids of carob powder oil may have resulted from the exposure of unsaturated fatty acids to air oxidation with the applied heat treatment.
Carob powder oil contains 40.45 oleic, 23.19 linoleic, 11.01 palmitic and 3.08% stearic acids [8]. The dominant fatty acids in the fatty acid composition of carob fruit powder oil were found to be similar to the fatty acids stated by Youssef et al. [8], but partial differences were observed in their amounts. These changes may possibly be due to location, ripening, the applied temperature and time, material structure, water amount, and extraction conditions. As a result, carob powder oils are rich in linoleic and linolenic acid, so they can be used in diets, for enrichment with essential fatty acids.

3.4. The Mineral Contents of Unroasted Carob Powder (raw) and Carob Powders Roasted at Different Temperatures

The mineral amounts of the raw and roasted (90, 120 and 150 °C) carob powders are displayed in Table 4. K, Ca, P, Mg, S, Na and Fe were the major elements of raw and roasted carob powders. The highest element was K, followed by Ca, P, Mg, S, Fe, Na, Pb, Cu, Zn B and Mn. in descending order.
While p values of the raw and roasted carob powders are assessed to be between 914.97 ± 117.60 (control) and 1091.75 ± 3 3.26 mg/kg (150 °C), K amounts of carob powder samples were found to be between 8889.40 ± 113.42 (control) and 10,606.93 ± 213.99 mg/kg (150 °C). Also, Ca and Mg values of the raw and roasted carob powders were altered, to be between 4362.82 ± 134.47 (control) and 4894.64 ± 99.26 mg/kg (120 °C) to 781.17 ± 50.84 (control) and 876.10 ± 17.32 mg/kg (150 °C), respectively. While S amounts of carob powder samples were found to be between 706.39 ± 34.35 (control) and 787.97 ± 36.32 mg/kg (120 °C), Na quantities of raw and roasted carob powders were altered to be between 196.05 ± 3.15 (control) and 235.87 ± 3.44 mg/kg (120 °C).
Fe quantities of the carob powders were assigned to be between 301.93 ± 6.76 (150 °C) and 394.76 ± 50.23 mg/kg (120 °C). The highest Cu (17.91 ± 5.14 mg/kg) and Zn (13.90 ± 2.13 mg/kg) were found in the control sample of carob powders. Also, Mn, Ni and B amounts of carob powders roasted at 120 °C temperature were at the highest levels (10.55 ± 0.53 mg/kg, 3.01 ± 0.02 mg/kg and 12.02 ± 0.07 mg/kg, respectively). Pb amounts in raw and roasted carob powders ranged from 26.29 mg/kg (150 °C) to 35.38 mg/kg (90 °C). Since Pb content is thought to be dangerous for human health, this Pb contamination may probably be caused by the environmental condition and soil structure and the roasting containers in which the carob grows. In general, the Pb contents of the roasted carob powders were low when compared to the control, and statistically significant changes were assigned among the results of raw and roasted carob powder samples (p < 0.05).
Carob powder is rich in Fe, Ca, Na, K, P and S [8]. The potassium content of carob fruits ranges from 970 mg/100 g to 1120 mg/100 g, while calcium content reaches 300 mg/100 g [12,35,36]. In carob powder, 10.28 Mn, 24.71 Zn, 381.80 Fe, 4.84 Cu, 9.79 Se, 2123.00 Na, 505.97 K, 8637.64 S, 2255.21 Ca and 17,577.80 mg/100 g P were found [37]. Ibrahim et al. [38] detected 864 ppm Ca, 66.90 ppm Fe, 12.70 ppm Mn, and 21.80 ppm Zn in seedless carob flour. In carob flour, 109.45 mg/kg A1, 72.05 mg/kg B, 4.41 mg/kg Ba, 6076.14 mg/kg Ca, 2.64 mg/kg Cu, 58.39 mg/kg Fe, 27 200.23 mg/kg K, 1.1 mg/kg Li, 1219.54 mg/kg Mg, 1.06 mg/kg Mn, 2052.56 mg/kg Na, 2.26 mg/kg Ni, 8500.94 mg/kg P, and 1.88 mg/kg Zn were found [39]. When the mineral contents of carob powder were compared with the literature data [8,37,38,39], it was determined that the predominant macro- and micro-elements were the same, and their amounts were partially different. In general, the Pb amounts of the roasted carob powders were low when compared to the control, and statistically significant changes were assigned among the results of raw and roasted carob-powder samples (p < 0.05). The reason for the increase in the mineral content of carob powders with heat treatment may probably be due to the decrease in the moisture quantity of the carob powder. Since carob powders are a very rich natural source of K, Ca, Mg and Fe elements, it is thought that they can be used as food supplements to increase the mineral content of most bakery products.

4. Conclusions

Some fluctuations in chemical and bioactive compounds and antioxidant activities of carob powders, depending on roasting temperatures, were observed. Both the moisture and oil quantities decreased, together with a roasting temperature increase. While total phenolic and flavonoid quantities of the roasted carob powders compared to control increased, the antioxidant activity values of the roasted carob powders decreased. The brightness of samples (L* values) showed a decrease after heat treatment, and the lowest L* value was monitored in sample roasted at 150 °C. Similar to results for the L* value, roasting temperature had a significant effect on both a* and b* values.
Gallic acid, 3,4-dihydroxybenzoic acid, catechin, rutin and ferulic acid were established at the highest quantities in raw and roasted carob powders. In general, the most observed increase in the amount of phenolic profiles was observed in carob powder roasted at 150 °C. The quantities of some phenolic constituents showed changes depending on the increase in temperature. Generally, the phenolic quantities of the carob powders roasted at 150 °C were higher than that of the control. Depending on the temperature and time, it can be said that the differences in phenolic profile quantities of carob powder dried at different temperatures were compared with the control group. Generally, the phenolic quantities of the carob powders roasted at 150 °C were higher than that of the control. Depending on the temperature and time, it can be said that the differences in phenolic profile quantities of carob powder dried at different temperatures were compared with the control group. The phenolic component quantities of the carob powders roasted at different temperatures increased significantly when compared to the control.
The highest quantities of saturated fatty acids were established in carob powder oil roasted at 90 °C. In general, the quantities of fatty acids in roasted carob powder oils at different temperatures compared to the control increased. However, the palmitic acid content of carob powder oil roasted only at 120 °C was higher than the palmitic acid quantity of carob powder oil roasted at both control and 90 and 120 °C.
The highest element was K, followed by Ca, P, Mg, S, Fe, Na, Pb, Cu, Zn B and Mn, in descending order. The protein quantity of the carob powder decreased with the heat treatment. In general, the Pb contents of the roasted carob powders were low when compared to the control, and statistically significant changes were assigned among the results for the raw and roasted carob powder samples (p < 0.05). High temperature roasting (150 °C) increased the bioactive properties and phenolic compound amounts of the carob powder. The carob powder can be used as a functional food additive in bakery products, due to the bioactive components, fatty acids, phenolic components and mineral contents it contains through roasting.

Author Contributions

Methodology, I.A.M.A. and M.M.Ö.; Software, F.Y.A.; Validation, I.A.M.A., F.Y.A. and E.K.; Formal analysis, M.M.Ö. and N.U.; Investigation, I.A.M.A. and M.M.Ö.; Data curation, F.Y.A. and E.K.; Writing—original draft, M.M.Ö.; Writing—review & editing, I.A.M.A., F.Y.A. and M.M.Ö. All authors have read and agreed to the published version of the manuscript.

Funding

The authors extend their appreciation to Researchers Supporting Project Number (RSPD2024R1074), King Saud University, Riyadh, Saudi Arabia.

Data Availability Statement

The original contributions presented in the study are included in the article, further inquiries can be directed to the corresponding author.

Conflicts of Interest

The authors declare no competing interests.

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Processes 12 01990 g001aProcesses 12 01990 g001b
Figure 1. Phenolic chromatograms of raw (control) and roasted (CP-90, CP-120, CP-150 °C) carob powders.
Figure 1. Phenolic chromatograms of raw (control) and roasted (CP-90, CP-120, CP-150 °C) carob powders.
Processes 12 01990 g001aProcesses 12 01990 g001b
Processes 12 01990 g002
Figure 2. Fatty acid chromatograms of raw (control) and roasted (at CP-90, CP-120 and CP-150 °C) carob powder oils.
Figure 2. Fatty acid chromatograms of raw (control) and roasted (at CP-90, CP-120 and CP-150 °C) carob powder oils.
Processes 12 01990 g002
Table 1. Physical–chemical properties of raw and roasted carob-powder samples.
Table 1. Physical–chemical properties of raw and roasted carob-powder samples.
TemperatureMoisture Content (%)Oil Content (%)L*a*b*
Control8.84 ± 0.13 ** a0.85 ± 0.15 a61.57 ± 1.28 a4.05 ± 0.35 d28.66 ± 0.32 a
90 °C4.14 ± 0.04 b ***0.40 ± 0.10 d60.24 ± 1.01 b4.32 ± 0.14 c26.25 ± 0.70 b
120 °C3.53 ± 0.39 c0.75 ± 0.05 b55.16 ± 1.38 c7.90 ± 0.10 b26.09 ± 0.80 c
150 °C3.34 ± 0.01 d0.50 ± 0.10 c45.08 ± 1.29 d11.23 ± 0.45 a24.59 ± 0.34 d
TemperatureTotal phenolic (mg/100 g)Total flavonoid (mg/100 g)Antioxidant activity (mmol/kg)Crude protein (%)
Control781.16 ± 17.85 d663.81 ± 32.12 d10.30 ± 0.01 a10.27 ± 0.54 a
90 °C869.63 ± 15.11 b747.62 ± 34.52 c10.27 ± 0.01 a8.87 ± 0.61 b
120 °C823.92 ± 75.51 c770.48 ± 41.49 b10.14 ± 0.02 b8.40 ± 0.87 c
150 °C903.07 ± 17.39 a1141.90 ± 37.49 a9.27 ± 0.049.45 ± 0.58 c
** Standard deviation; *** values within each column followed by different letters are significantly different at p < 0.05.
Table 2. Phenolic compounds of raw and roasted carob-powder samples.
Table 2. Phenolic compounds of raw and roasted carob-powder samples.
Phenolic Compounds (mg/100 g)Control90 °C120 °C150 °C
Gallic acid45.16 ± 0.40 * d108.39 ± 6.19 c115.13 ± 6.09 b120.66 ± 9.30 a
3,4-Dihydroxybenzoic acid7.06 ± 0.83 d **8.55 ± 1.52 c11.13 ± 1.65 b20.46 ± 2.96 a
Catechin13.65 ± 0.81 d61.02 ± 1.59 b58.39 ± 0.98 c68.86 ± 1.30 a
Caffeic acid2.56 ± 0.45 c2.23 ± 0.53 d18.67 ± 4.61 a11.90 ± 0.69 b
Syringic acid3.69 ± 1.00 c1.95 ± 0.43 d33.47 ± 9.25 a24.17 ± 1.89 b
Rutin16.79 ± 3.04 d31.81 ± 0.82 c37.82 ± 0.95 b39.63 ± 0.57 a
p-Coumaric acid2.58 ± 0.17 d2.80 ± 0.25 c3.75 ± 0.77 b8.99 ± 1.70 a
Ferulic acid6.81 ± 0.87 c4.19 ± 0.70 d9.90 ± 0.58 b10.25 ± 1.80 a
Resveratrol0.35 ± 0.04 d2.63 ± 0.84 a2.14 ± 0.32 c2.40 ± 0.22 b
Quercetin0.83 ± 0.05 d2.14 ± 0.63 c6.27 ± 1.13 a4.07 ± 0.26 b
Cinnamic acid1.81 ± 0.31 d1.97 ± 0.27 c2.32 ± 0.32 a1.29 ± 0.35 b
Kaempferol0.26 ± 0.01 c0.49 ± 0.04 b0.54 ± 0.06 a0.22 ± 0.03 d
* Standard deviation; ** values within each row followed by different letters are significantly different at p < 0.05.
Table 3. Fatty acid composition of the oils extracted from raw and roasted carob-powder samples.
Table 3. Fatty acid composition of the oils extracted from raw and roasted carob-powder samples.
Fatty Acids (%)Control90 °C120 °C150 °C
Myristic0.13 ± 0.00---
Palmitic10.02 ± 0.06 * d16.19 ± 0.18 a12.73 ± 0.00 b11.93 ± 0.02 c
Stearic6.58 ± 0.02 b **5.19 ± 0.02 d8.41 ± 0.01 a5.87 ± 0.01 c
Oleic29.55 ± 0.02 d36.27 ± 0.10 a35.66 ± 0.03 b30.30 ± 0.01 c
Linoleic17.30 ± 0.02 d36.99 ± 0.06 a19.78 ± 0.07 c23.80 ± 0.00 b
Arachidic0.35 ± 0.00 d0.75 ± 0.01 a0.48 ± 0.00 b0.46 ± 0.00 c
Linolenic35.70 ± 0.12 b46.17 ± 0.09 a22.39 ± 0.16 d27.29 ± 0.00 c
Behenic0.27 ± 0.01 d0.32 ± 0.01 c0.37 ± 0.02 a0.35 ± 0.00 b
* Standard deviation; ** values within each row followed by different letters are significantly different at p < 0.05.
Table 4. Mineral contents of raw and roasted carob powders (mg/kg).
Table 4. Mineral contents of raw and roasted carob powders (mg/kg).
Roasting TemperaturesPKCaMgSNaFeCuMnNiPbZnB
Control914.97 ± 117.60 * d8889.40 ± 113.42 d4362.82 ± 134.47 d781.17 ± 50.84 d706.39 ± 34.35 d196.05 ± 3.15 d373.24 ± 15.93 b17.91 ± 5.14 a9.91 ± 0.88 b2.48 ± 0.47 d29.31 ± 7.73 c13.90 ± 2.13 a10.85 ± 0.13 d
90 °C97,392 ± 253.24 c **9719.97 ± 776.33 c4528.77 ± 207.31 c817.80 ± 63.89 c723.65 ± 90.49 c222.42 ± 4.52 b371.67 ± 93.77 c13.97 ± 0.07 d8.96 ± 0.02 d2.50 ± 0.49 c35.38 ± 3.56 a11.97 ± 0.97 d11.94 ± 0.03 b
120 °C1032.63 ± 88.65 b10,275.55 ± 533.05 b4894.64 ± 99.26 a866.39 ± 11.02 b787.97 ± 36.32 a235.87 ± 3.44 a394.76 ± 50.23 a15.00 ± 0.05 b10.55 ± 0.53 a3.01 ± 0.02 a31.47 ± 0.56 b12.49 ± 0.52 b12.02 ± 0.07 a
150 °C1091.75 ± 33.26 a10,606.93 ± 213.99 a4849.76 ± 210.57 b876.10 ± 17.32 a783.92 ± 23.54 b212.06 ± 4.00 c301.93 ± 6.76 d13.89 ± 0.04 d9.43 ± 0.48 c2.97 ± 0.01 b26.29 ± 5.39 d11.89 ± 0.03 e11.89 ± 0.03 c
* Standard deviation; ** values within each column followed by different letters are significantly different at p < 0.05.
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Mohamed Ahmed, I.A.; AlJuhaimi, F.Y.; Özcan, M.M.; Uslu, N.; Karrar, E. The Role of Different Roasting Temperatures on the Physico-Chemical Properties, Phenolic Compounds, Fatty Acid and Mineral Contents of Carob (Ceratonia siliqua L.) Fruit Powder. Processes 2024, 12, 1990. https://doi.org/10.3390/pr12091990

AMA Style

Mohamed Ahmed IA, AlJuhaimi FY, Özcan MM, Uslu N, Karrar E. The Role of Different Roasting Temperatures on the Physico-Chemical Properties, Phenolic Compounds, Fatty Acid and Mineral Contents of Carob (Ceratonia siliqua L.) Fruit Powder. Processes. 2024; 12(9):1990. https://doi.org/10.3390/pr12091990

Chicago/Turabian Style

Mohamed Ahmed, Isam A., Fahad Y. AlJuhaimi, Mehmet Musa Özcan, Nurhan Uslu, and Emad Karrar. 2024. "The Role of Different Roasting Temperatures on the Physico-Chemical Properties, Phenolic Compounds, Fatty Acid and Mineral Contents of Carob (Ceratonia siliqua L.) Fruit Powder" Processes 12, no. 9: 1990. https://doi.org/10.3390/pr12091990

APA Style

Mohamed Ahmed, I. A., AlJuhaimi, F. Y., Özcan, M. M., Uslu, N., & Karrar, E. (2024). The Role of Different Roasting Temperatures on the Physico-Chemical Properties, Phenolic Compounds, Fatty Acid and Mineral Contents of Carob (Ceratonia siliqua L.) Fruit Powder. Processes, 12(9), 1990. https://doi.org/10.3390/pr12091990

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