Freeze-drying and oven drying on the nutritional and functional properties of fresh and pre-cooked Xanthosoma taioba leavesABSTRACT
Unconventional food plants (UFPs) are sustainable alternatives for diversifying diets and enhancing the value of Brazilian socio-biodiversity. The nutritional and functional potential of taioba (Xanthosoma taioba E.G. GONÇ.), a UFP, has not been determined. This study aimed to evaluate the nutritional, phytochemical, antioxidant, and aromatic compound profiles of taioba leaves cultivated in a syntropic system in Santo Antônio do Tauá, Pará, Brazil. The taioba leaves were subjected to freeze drying or oven drying with and without prior cooking. This study examined the macronutrients, minerals (inductively coupled plasma optical emission spectroscopy), phenolic compounds, antioxidant activity (2,2-diphenyl-1-picrylhydrazyl, 2,2’-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid), and ferric reducing antioxidant power assays), pigments, color profile, phenolic profile (high-performance liquid chromatography), and volatile compounds (gas chromatography tandem mass spectrometry) in processed taioba leaves. The contents of proteins, insoluble fiber, calcium, and iron were up to 26 g/100 g, 18.44-20.79 g/100 g, 920 mg/100 g, and 30 mg/100 g, respectively. The raw samples exhibited enhanced antioxidant activity and total phenolic contents, indicating the thermal sensitivity of these compounds. The volatile profile markedly varied between the processing methods. Freeze drying preserved alcohols and ketones associated with fruity and herbaceous notes, while oven drying preserved aldehydes and acids associated with oxidation and thermal degradation. Compounds, such as acetoin, promoted the technological and sensory potential of taioba. Thus, the favorable nutritional and functional properties of X. taioba can be harnessed for its application as a food ingredient, improving sustainable agri-food systems and conserving Amazonian biodiversity.
Index terms:
Phenolic compounds; volatile compounds; antioxidant capacity; food processing
RESUMO
Plantas Alimentícias Não Convencionais (PANC) representam alternativas sustentáveis para diversificar a alimentação e valorizar a sociobiodiversidade brasileira. Entre elas, a taioba (Xanthosoma taioba E.G. GONÇ.) destaca-se como uma espécie pouco explorada, com elevado potencial nutricional e funcional. Este estudo teve como objetivo avaliar os perfis nutricional, fitoquímico, antioxidante e de compostos aromáticos de folhas de taioba cultivadas em sistema sintrópico em Santo Antônio do Tauá, Pará, Brasil, e submetidas a diferentes métodos de processamento: liofilização e secagem em estufa, com e sem cozimento prévio. As análises incluíram a determinação de macronutrientes, minerais por ICP-OES, compostos fenólicos e atividade antioxidante (DPPH, ABTS, FRAP), pigmentos, cor instrumental, perfil fenólico por HPLC e compostos voláteis por CG-MS. Os resultados revelaram teores relevantes de proteínas (até 26 g/100 g), fibras insolúveis (18,44-20,79 g/100 g) e minerais como cálcio (até 920 mg/100 g) e ferro (até 30 mg/100 g). A atividade antioxidante e o teor de fenólicos totais foram maiores nas amostras não submetidas ao cozimento, indicando a sensibilidade térmica desses compostos. O perfil de compostos voláteis apresentou diferenças marcantes entre os métodos de processamento: a liofilização preservou álcoois e cetonas associados a notas frutadas e herbáceas, enquanto a secagem em estufa intensificou aldeídos e ácidos relacionados à oxidação e à degradação térmica. Compostos como a acetoína reforçam o potencial tecnológico e sensorial da taioba. Em conclusão, essa espécie apresenta propriedades nutricionais e funcionais relevantes, sustentando seu uso como ingrediente alimentar e contribuindo para sistemas agroalimentares sustentáveis e para a conservação da biodiversidade amazônica.
Termos para indexação:
Compostos fenólicos; compostos voláteis; capacidade antioxidante; processamento de alimentos
Introduction
Brazil has one of the richest biodiversity of plant species, accounting for approximately 15%-20% of the global plant diversity. This vast biodiversity also includes unconventional food plants (UFPs) (Borges & Silva 2018), which have one or more edible parts. UFPs are often not part of the diet of the population and occur spontaneously or are cultivated. Additionally, UFPs are referred to as weeds or spontaneous herbs (Liberato, Lima & Silva 2019; Minello et al., 2021). Although UFPs have garnered scientific and commercial interest, the technological and functional profiles of these species, especially the stability of their bioactive compounds under different processing conditions, have not been characterized.
The nutritional composition of UFPs meets consumer demand for healthy foods. UFPs comprise bioactive compounds with potential applications in the food, chemical, and pharmaceutical industries. The incorporation of UFPs into food formulations can provide nutritional and sensory benefits, aligning with the market trend toward plant-based products (Milião et al., 2022; Pinela, Carvalho & Ferreira, 2017). Recent studies have demonstrated that plant-derived bioactive compounds may exhibit health-promoting properties, contributing to disease prevention and management by interacting with molecular targets and modulating physiological processes (Cheng et al., 2023). Plant-derived bioactive compounds are reported to decrease the risk of chronic non-communicable diseases, indicating their importance for public health (Frumuzachi et al., 2025).
The growing competition in the food sector has driven the development of healthy products with unique qualities and sustainable profiles. The technological innovations involving the use of natural plant-derived products have piqued the interest of the scientific community. For example, volatile organic compounds, which contribute to food aroma and may provide health benefits, are considered natural alternatives to chemical additives (Derbassi et al., 2022). Thus, aromatic compounds have increasingly been recognized as key flavor components with potential applications in the food industry (Gong et al., 2023).
Among the several UFP species in Brazil, Xanthosoma taioba E.G. Gonç. (popularly called “taioba”) is a tuberous herbaceous plant belonging to the Araceae family. The other names of taioba include “taioba-verde,” “taiá,” “inhame-de-folha,” “macabo,” “mangará,” “tannia,” and “yautia” (Kinupp & Lorenzi, 2021). In addition to its nutritional value, taioba presents technological potential for application in food systems, especially in the development of plant-based products, owing to its functional properties and phytochemical composition.
The productive potential of the rich Amazonian biodiversity in promoting food security, regional development, and a sustainable forest-based economy has been underexplored. Tourneau (2025) revealed that some forest products have reached market relevance. However, several other forest products are underutilized due to challenges related to logistics, infrastructure, and public policies. Research on the leaves of taioba, which is cultivated in Amazonian agroforestry systems, may open new opportunities to enhance socio-biodiversity, expand dietary diversity, and encourage the sustainable use of native species. The adoption of syntropic systems may influence plant physiological and qualitative attributes due to optimized use of light, water, and nutrients, as well as the high biological diversity and ecological interactions within the cultivation system (Jacobi et al., 2025).
The cultivation of taioba is limited when compared with that of staple crops, such as maize, sorghum, and cassava. However, taioba cultivation is associated with high productivity (30 t/ha), low production cost, and ease of cultivation (Serna-Loaiza, Carmona-Garcia & Cardona, 2018). The leaves of Xanthosoma species have nutritional and functional benefits (Ukom, Nwanagba & Okereke, 2020). However, Xanthosoma leaves are underutilized at both industrial and domestic levels, with their use restricted primarily to areas of cultivation. Furthermore, processing technologies, especially drying technologies, have a critical role in preserving the beneficial attributes of Xanthosoma leaves, influencing the stability of phytochemical compounds and sensory characteristics. Recent studies have demonstrated that different drying methods significantly alter the metabolite profiles and antioxidant activity. Techniques, such as freeze drying, can preserve the bioactive compound, color, and flavor profiles of plant products (Uwineza & Zhang, 2026).
Although taioba has been taxonomically identified, studies on taioba leaves are limited (Gonçalves, 2011). X. taioba is often confused with X. sagittifolium and X. robustum. In contrast to X. sagittifolium and X. robustum, X. taioba exhibits a hypogeal stem in mature individuals and pale pink (rather than pure white) staminodes. X. taioba can also be distinguished from X. sagittifolium based on its discolored primary lateral veins and the absence of sagittate venation in young leaves. Meanwhile, X. taioba can be distinguished from X. robustum based on its non-sagittate young leaves and the consistent absence of a bare portion on the basal ribs. Additionally, X. taioba can be distinguished from X. mafaffa based on its small size and lack of a basal rib (Gonçalves, 2011).
Several studies have reported that unconventional plant-based food sources can be integrated into food chains with reduced environmental impacts. UFPs are gaining increasing visibility among consumers seeking healthy and sustainable diets. Species of the genus Xanthosoma comprise macronutrients and bioactive compounds with antioxidant capacity and potential applications in disease prevention (Jesus Benevides et al., 2022). However, limited studies have evaluated the effects of different processing methods on the nutritional, phytochemical, and aromatic profiles of Xanthosoma species.
This study aimed to evaluate the nutritional, phytochemical, antioxidant, and volatile compound profiles of taioba leaves cultivated in a syntropic system. To the best of our knowledge, this is the first study to characterize the volatile compound profile of X. taioba leaves. Previous studies have predominantly focused on the nutritional composition and phenolic compounds of X. taioba. In contrast, this study investigated the volatile compounds of taioba leaves to determine the functional potential of this species. Therefore, this study provides pioneering insights into the aromatic composition of taioba and compares the profiles of taioba with those of other unconventional food plants, broadening the perspectives for the technological valorization of this species. This study hypothesized that drying methods significantly affect the preservation of bioactive and volatile compounds in taioba leaves, influencing their functional properties and potential applications in food products.
Material and Methods
Plant material and sample processing
This study was conducted in a cultivation area with a syntropic farming system. The leaf samples were collected between December 2023 and January 2024. The study site is located in the municipality of Santo Antônio do Tauá, Pará, Brazil, at a location known as Horta da Terra (coordinates: −1.0552°, −48.1268°).
Taioba was identified through the preparation of an exsiccate specimen (registration number IAN 202.755) and deposited in the Herbarium of Embrapa-Eastern Amazon. The collected leaves were immediately placed in low-density polyethylene plastic bags, stored in a cooler, and transported to the Physical Chemistry Laboratory at IFPA-Castanhal Campus. The leaves were sanitized in a 100-ppm sodium hypochlorite solution for 10 min and rinsed with water. The samples were classified into the following groups: FTCRL group: raw leaves subjected to freeze drying at −51°C for 48 h using a freeze-dryer (LIOBRAS, L101, São Paulo, Brazil); FTCRD, raw leaves subjected to air-drying at 40°C for 48 h using a circulating oven (TE-395, Tecnal, São Paulo, Brazil); FTCOZL, cooked leaves subjected to freeze-drying at −51°C for 48 h; FTCOZD, cooked leaves subjected to air-drying at 40°C for 48 h.
The dried leaves were ground using a knife mill (SOLAB, SL-30, São Paulo, Brazil) to obtain a homogeneous powder. The cooking process aimed to reduce the antinutritional factor (calcium oxalate) and ensure safe consumption. The leaves were cooked in an aluminum container with water (1:5; w/v) at 100°C for 40 min. Next, the leaves were rapidly cooled in ice water to stop the cooking process and dried using absorbent paper. Some samples were freeze-dried at −51°C for 48 h and ground in a mill to obtain a homogeneous powder. The remaining samples were dehydrated in an oven with air circulation at 45°C for 48 h and ground using the same method as described for the freeze-dried samples.
Chemical, nutritional, and phytochemical profile analyses
The centesimal composition analyses were performed (based on dry weight) at the Labfood Laboratory of the Federal University of Goiás (UFG), following the standard methods of the Official Methods of Analysis (AOAC) (Association of Official Agricultural Chemists - AOAC, 2005). The following parameters were analyzed based on the standard methods of the Official Methods of Analysis (AOAC, 2019): moisture, ash, soluble, insoluble, total dietary fiber contents, protein, carbohydrate, and lipid contents. The total energy value was estimated considering the conversion factors of 4 kcal/g for proteins and carbohydrates and 9 kcal/g for lipids. All analyses were performed in quintuplicate.
The mineral contents (Ca, K, Na, P, Cu, Fe, Mg, Mn, and Zn) were determined after the acid digestion of the samples, following previously reported methods (Melo & Silva, 2008). This study analyzed the mineral contents using an inductively coupled plasma optical emission spectrometry (ICP-OES) system (Shimadzu ICPE-9000).
The extract used to estimate the content of phenolic compounds and antioxidant activity was prepared as described previously (Rubio et al., 2022) with minor modifications. Briefly, the powdered sample (2 g) was mixed with 50 mL of 70% (v/v) ethanol in a 150-mL Erlenmeyer flask. The mixture was subjected to extraction for 30 min in an ultrasonic bath (Digital Ultrasonic Cleaner, model D409X, CTA) at room temperature. Next, the mixture was transferred to a 2-mL Eppendorf tube and centrifuged at 10,000 rpm for 10 min using a microcentrifuge (model K14-1215P, KASVI). The supernatant was filtered through a hydrophilic nylon syringe filter (diameter: 25 mm; pore size: 0.45 μm). The filtrate was collected in a clean container and stored at 5°C in the dark until analysis. Before analysis, the extract was diluted to adjust the concentration within the absorbance range of the standard curve.
To determine the total phenolic content, the extract (0.25 mL) was mixed with 2.75 mL of Folin-Ciocalteu reagent in test tubes wrapped in aluminum foil and vortex-mixed for 10 s. The mixture was left undisturbed for 5 min and incubated with 0.25 mL of sodium carbonate solution at room temperature in the dark for 1 h. The absorbance of the reaction mixture at 725 nm was measured using a UV-visible spectrophotometer (Shimadzu, UV 1800). The results are expressed as gallic acid equivalent (GAE). The total phenolic contents were determined from the standard curve (20-100 mg GAE/100 g) (Genovese et al., 2008). The Folin-Ciocalteu method provides an estimate of total reducing compounds but is not specific to phenolic compounds.
The capacity of the extract to scavenge the free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) was determined following the previously reported method (Sánchez-Moreno, Larrauri & Saura-Calixto, 1998). The calibration curve was generated using a Trolox standard solution (0-1000 μmol/L) (R² = 0.999). The absorbance of the reaction mixture at 517 nm was determined. The DPPH scavenging activity of the sample was calculated based on the absorbance values. The Trolox equivalent (TE) was determined.
The 2,2’-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) free radical (ABTS•+) scavenging activity was determined following previously reported methods (Rufino et al., 2007). The stock solution of ABTS•+ was prepared by mixing 5 mL of ABTS stock solution (7 mmol/L) with 88 μL of potassium persulfate (140 mmol/L). The mixture was then diluted with 70% ethanol until the absorbance reached 0.70 ± 0.05 at 734 nm. To generate the standard curve (R² = 1), the ABTS radical scavenging activity of Trolox (100 to 2000 μmol/L) was calculated. The percentage inhibition of ABTS radicals was determined using the following equation: Percentage inhibition of ABTS = [(Control absorbance − final absorbance of the Trolox + ABTS mixture)/Control absorbance]. The results are expressed as μmol Trolox per liter (μmol/L) and subsequently converted to μmol of TE per gram of sample, considering the sample weight, solvent volume, and dilution factors used to prepare the extracts.
The ferric reducing powder (FRAP) assay was performed following previously reported methods (Rufino et al., 2007) with slight modifications. A Trolox stock solution (1600 μmol/L) was used to prepare standard working solutions (0-800 μmol/L) for generating the standard curve (R² = 0.999). The absorbance of the samples at 595 nm was measured. The antioxidant activity of the extract was calculated from the Trolox standard curve. The results are expressed as μmol TE/L and converted to μmol TE/g of sample using the same considerations as above.
Next, this study determined the contents of total chlorophylls and carotenoids. The sample (approximately 0.5 mg) was mixed with 10 mg of MgCO₃ and 10 mL of acetone in a 2-mL Eppendorf tube. The tubes were sealed with screw caps, and the mixture was vortex-mixed using a Wizard Advanced IR Vortex Mixer (Velp Scientifica, Usmate, Italy) at 2,000 rpm. The samples were then subjected to ultrasonication using an ultrasonic bath (Digital Ultrasonic Cleaner, model D409X, CTA, Brazil) under the following conditions: frequency, 40 kHz; power, 400 W; duration, 10 min. The sonicated samples were centrifuged at 13,700 rpm for 10 min in a microcentrifuge (model K14-1215P, KASVI, Brazil). The supernatant was filtered using a hydrophilic nylon syringe filter (diameter: 25 mm; pore size: 0.45 µm) and transferred to clean containers.
Carotenoids and chlorophylls are highly photosensitive. To minimize the photodegradation of these pigments, all extractions and analyses were performed under low-light conditions. Five replicates were established for each sample to ensure maximum absorbance values of 1.00 absorbance unit (Hynstova et al., 2018). The absorbance was measured using a spectrophotometer at specific wavelengths (662 nm for chlorophyll a, 645 nm for chlorophyll b, and 470 nm for total carotenoids, and 653 nm and 654 nm), following the previously reported methods (Lichtenthaler 1987).
The color profile of the samples was evaluated using a colorimeter (Color Flex EZ/HunterLab, USA). The L* value, ranging from 0 (black) to 100 (white), indicates the sample lightness. The a* and b* values were used to calculate the chroma (C*) value (a*: color scale from green (−60) to red (+60); b* color scale from blue (−60) to yellow (+60)). Color saturation and intensity were calculated as chroma, following the method described in AACC 14-22 (2006). The colorimeter was calibrated before analysis using the white calibration plate from Konica Minolta.
Qualitative profiling of phenolics using high-performance liquid chromatography (HPLC)
The phenolic compounds were quantified using a Thermo Scientific Ultimate 3000 Liquid Chromatograph and a Thermo Scientific Q-Exactive High Resolution Mass Spectrometer under the following conditions: column, Agilent C18 column (4.6 × 100 mm; 3 μm); ion source, heated electrospray ionization; mode, negative; spray voltage, 3.5 kV; sheath gas, 30 arbitrary units; auxiliary gas, 10 arbitrary units; capillary temperature, 350°C; auxiliary gas temperature, 250°C; tube lens, 55; mass range, m/z 150-1200; mobile phase A, deionized water acidified with 0.1% formic acid (mobile phase A) and mobile phase B, methanol acidified with 0.1% formic acid. The gradient program was as follows: 93:07 (A:B), followed by 70:30 (A:B) over 10 min, 50:50 (A:B) in 5 min, 30:70 (A:B) in 3 min, 20:80 (A:B) in 2 min, and 100% B for 3 min, and a final 22-min equilibration.
Gas chromatography mass spectrometry (GC-MS)
Volatile compounds were analyzed using a Shimadzu Nexis GC2030 gas chromatograph coupled to a Shimadzu QP2020 NX mass spectrometer equipped with a SH-Stabilwax-MS column (30 m × 0.25 mm × 0.25 µm). Before analysis, the samples were heated in the headspace at 80ºC for 30 min. The sample (2 g) was injected into the chromatograph and analyzed under the following conditions: mode, split less; oven temperature, initially set to 40°C, followed by 160°C at 5°C/min (held for 5 min), 200°C at 10°C/min (held for 5 min), and 250°C; total analysis time, 32-38 min (due to the dielectric property (DEP) detection peak); carrier gas, helium 5.0; pressure, 4.7 psi; flow rate, 13.4 mL/min; linear velocity, 35 cm/s; injector interface and ion source temperature, 250°C. The retention time for the DEP peak was 32.8 min. The settings for the mass spectrometer were as follows: modes, scan mode (range 25-500 Da) and single ion monitoring mode (m/z: 149, 177, and 122); voltage, 70 eV; ion source, electron ionization.
Statistical analyses
The normality and homogeneity of variance of the data were assessed. Means were compared using analysis of variance, followed by Tukey’s post-hoc test. Differences were considered significant at p < 0.05. The similarities in nutrient content, phytochemicals, antioxidant activity, and color parameters were assessed using principal component analysis (PCA). All statistical analyses were performed using R software (R Core Team (2024).
Results and Discussion
Centesimal composition, color index, mineral content, phenolic compounds, antioxidants, and pigments
The average values (mg/100 g) for the centesimal composition and color index of taioba leaves are shown in Table 1.
Fresh leaves undergo rapid deterioration and are consequently unsuitable for long-term storage. However, the findings of this study indicated that the stability of leaves improved with processing, extending the shelf life for several months.
Carbohydrates, proteins, and dietary fiber were the most abundant macronutrients in the samples. The carbohydrate content in powdered taioba leaves reported in this study was lower than the values reported by Santos et al. (2021) for freeze-dried taioba leaves (66.64 g/100 g) (Santos et al., 2021) but higher than the values reported by Leterme et al. (2025) for taioba leaves (19.7-22.9 g/100 g) (Leterme et al., 2005). These differential carbohydrate contents can be attributed to different drying techniques and the method used to calculate the content on a dry weight basis.
UFPs have potential applications in the food industry owing to their high protein content. Proteins are distributed in different plant parts, especially in the leaves. The concentrations of proteins range from 20% to 37%, depending on the species. Thus, UFPs exhibit a higher protein content (on a dry weight basis) than traditional crops, such as rice and wheat (Milião et al., 2022).
As shown in Table 1, samples in the FTCRL group exhibited the highest protein content, which can be attributed to the processing method that may have enhanced protein solubility (Ezeocha, Ojimelukwe & Gi, 2012). In contrast, samples in the FTCOZD group exhibited the lowest protein content.
The lipid levels in the samples ranged from 5.75 ± 0.11 to 3.53 ± 0.03. Additionally, the lipid levels were significantly different between the cooked and raw samples.
(Timm et al., 2023) revealed that cooking does not consistently affect fiber content. The elimination of water during cooking increases the total fiber content in the cooked product when compared with that in the fresh product. However, this study demonstrated that hydrothermal treatment slightly reduced the fiber content.
Processing methods do not exert consistent effects on soluble and insoluble fiber contents. Legumes are rich in soluble fiber, whereas plant-based protein isolates, such as those from soy and pea, are rich in insoluble fiber. The dietary fiber content in dried fruits is higher than that in fresh fruits, which can be attributed to water loss during processing (Timm et al., 2023).
Both cooking and drying significantly altered the color parameters (p < 0.05). The L* (lightness), a* (red-green), b* (yellow-blue), and chroma values were high in the raw leaves but were low in cooked samples (Table 1).
In humans, minerals are involved in several essential processes, including bone formation and nerve signal transmission, supporting a healthy metabolism. The mineral contents significantly (p < 0.05) varied between the groups (Table 2).
The calcium levels in cooked samples were higher than those in raw samples. This can be attributed to the hydrothermal treatment-mediated release of calcium previously complexed with oxalates in the plant matrix (Maila & Tseke, 2024). Additionally, the leaching of calcium during cooking is lower than that of soluble minerals, such as potassium. This is because calcium is strongly associated with plant tissues (Ho & Redan, 2022). Therefore, the increased calcium contents reflect enhanced calcium retention and relative availability rather than an absolute increase in its content. Oxalates in some vegetables bind to calcium, forming insoluble salts that are not absorbed by the gastrointestinal tract. Thus, calcium bioavailability is inversely proportional to the oxalate concentration in food (Shkembi & Huppertz, 2021).
Taioba leaves exhibited upregulated calcium levels (Table 2). Consistently, previous studies (Muleya, Bailey & Bailey, 2024) have reported enhanced calcium levels in steamed cabbage leaves (959 ± 121 mg/100 g). However, the calcium content in this study was lower than that reported by Pathan et al. (2019) (2,597 mg/100 g) (Pathan et al., 2019) in amaranth leaves. The high calcium levels in taioba leaves can contribute to a healthy diet.
FTCRL and FTCOZD samples exhibited high magnesium contents (210.24 ± 0.54 and 176.84 ± 1.15 mg/100 g, respectively). These magnesium contents are significantly higher than those reported by Sayeed et al. (2021) in Colocasia esculenta leaves (64 ± 5.05 mg/100 g) and water spinach (21 mg/100 g) (Sayeed et al., 2021).
Iron in plant-based foods occurs predominantly in the non-heme form, whereas that in animal-derived foods occurs in heme form. The bioavailability of the non-heme iron is low. Additionally, the absorption of non-heme iron is dependent on dietary components, such as phytates, polyphenols, and oxalates.
Powdered taioba leaves can serve as an excellent source of calcium (Ca), magnesium (Mg), iron (Fe), zinc (Zn), manganese (Mn), and copper (Cu) when compared with other widely consumed leafy vegetables.
As shown in Table 3, both FTCRL and FTCRD samples exhibited potent DPPH radical scavenging activities. In contrast, both FTCOZL and FTCOZD samples exhibited decreased DPPH radical scavenging activities. This suggests that cooking decreases the DPPH radical scavenging activity of taioba leaves. Antioxidants reduce DPPH radicals primarily through hydrogen atom transfer. Additionally, DPPH radicals are relatively stable and can be neutralized by reactive reducing agents, such as phenolic compounds, polyphenols, and flavonoids (Morabbi Najafabad & Jamei, 2014).
Santos et al. (2021) reported that the DPPH scavenging activity of taioba leaves cooked for 10 min and subjected to freeze drying was 27.35 ± 0.77 µg TE/g (Santos et al., 2021). In this study, the ABTS scavenging activity of taioba leaves was low, which may be due to the prolonged cooking time (40 min at 100°C). The ABTS scavenging activity was significantly different between the FTCRD and FTCOZD groups. Benevides et al. revealed that the FRAP values of X. sagittifolium leaves, petiole, and whole plant were 0.0213, 0.0114, and 0.0144 µM, respectively (Jesus Benevides et al., 2022). These values were higher than those reported for taioba leaves in this study. Roslan et al. (2020) examined the effect of drying methods on the antioxidant properties of tea leaves (Camellia sinensis). The authors reported that the FRAP values in freeze-dried leaves are higher than those in conventionally oven-dried leaves (5.07 ± 0.01 vs. 2.07 ± 0.01 mM Fe²⁺/g dry weight) (Roslan et al., 2020).
In this study, the cooking method significantly affected the total phenolic content (p < 0.05). The mean total phenolic contents of FTCRL and FTCRD samples were 30.18 ± 0.99 and 35.15 ± 0.54 mg GAE/100 g, respectively, which were higher than those in cooked taioba leaves. The decreased phenolic content in cooked samples can be attributed to changes in the matrix components, such as the degradation of tissue structure during cooking (Zor et al., 2022).
Cooking also decreases the phenolic content in other vegetables. De Rosso et al. evaluated bioactive compounds and antioxidant activity in kale and red cabbage (Murador, Mercadante & Rosso, 2016). The authors reported that the levels of bioactive compounds and antioxidants in boiled samples were significantly lower (31%, p < 0.001) than those in raw samples. This can be attributed to the loss of phenolic compounds through leaching into the cooking water. Cooking softens plant tissues, facilitating the release of phenolic compounds from the cellular matrix of the food (Blessington et al., 2010).
In this study, the cooked taioba leaves exhibited downregulated carotenoid contents. This can be attributed to the simultaneous release and degradation of carotenoids during food processing. Carotenoids are released due to tissue rupture during processing and undergo degradation due to chemical reactions, such as oxidation and isomerization (Wang et al., 2023).
In the freeze-dried samples, the proportion of chlorophyll a was approximately three times higher than that of chlorophyll b. Meanwhile, the proportion of chlorophyll a was approximately 2.5 times higher than that of chlorophyll b in oven-dried samples. These findings are consistent with previous work (Santos et al., 2021), reporting that the total chlorophyll content in lyophilized X. taioba E.G leaves was 7.54 ± 0.52 mg/100 g.
The Folin-Ciocalteu reagent is not specific to phenolic compounds but may also react with other reducing substances in the food matrix. This study did not remove proteins before analysis. Thus, the total phenolic content reported in this study should be interpreted as an estimate of reducing compounds associated with the phenolic fraction rather than a specific quantification of individual phenolic compounds.
Cooking may promote the loss of phenolic compounds through both thermal degradation and leaching. This study did not examine the phenolic content in the cooking water. Thus, the relative contribution of these mechanisms was not distinguished, representing a limitation of the study. Although the treatments were compared as independent conditions, the potential interaction between cooking and drying methods was not examined using a two-factor experimental design.
Multivariate discrimination of centesimal composition parameters, color index, minerals, phenolic compounds, antioxidants, and pigments
The characteristics of the treatment groups were examined by reducing the dataset based on each parameter studied.
The first two principal components explained 81.11% of the variation. In particular, principal component 1 (PC1) and PC2 explained 50.68% and 30.43% of the variations, respectively (Figure 1). These results indicate that cooking followed by drying exerted distinct effects, highlighting the impact of the processing method used for leaf drying. PC1 and PC2 captured most of the variability in the dataset, providing a robust summary of the effects of processing on the nutritional, physicochemical, and functional attributes of taioba leaves.
As shown in Figure 1, X. taioba leaves subjected to freeze drying and conventional drying processes were grouped into four distinct clusters without notable outliers. The parameters analyzed exhibited distinct clustering based on the treatment groups. In PC1, samples from the FTCRL, FTCRD, and FTCOZD groups exhibited close clustering. PC2 comprised the samples from the FTCOZL group. These clustering patterns indicate that the combination of cooking and freeze drying contributed to the most distinct physicochemical and functional profile among the evaluated treatments, suggesting a pronounced effect of this processing combination on the preservation and concentration of specific compounds.
component analysis (PCA) based on the types of drying method in taioba leaves. clo T, total chlorophyll; clo A chlorophyll a; clo B, chlorophyll b; CRO, chroma; CAR, carotenoids; FET, total phenolics; FT, total fiber; FS, soluble fiber; FI, insoluble fiber; VE, energy value; FTCRL, freeze-dried raw taioba leaf samples; FTCOZL, freeze-dried cooked taioba leaf samples; FTCRD, raw oven-dried taioba leaf samples; FTCOZD, oven-dried cooked taioba leaf samples.
In PC1, the variables exhibiting positive correlation included phosphorus (P), insoluble fiber, ABTS scavenging activity, and total phenolics. The clustering of total phenolics with ABTS scavenging activity suggests that the ABTS scavenging activity was strongly associated with compounds that can scavenge radicals through electron-transfer mechanisms, reflecting the contribution of phenolic compounds preserved in these treatments. The positive association with insoluble fiber may also indicate the retention of structural components within the plant matrix that can interact with or retain phenolic compounds in the tissue.
In PC2, the strongly correlated variables were calcium (Ca), manganese (Mn), carbohydrates, color (L*), chroma, carotenoids, FRAP value, and DPPH scavenging activity. These parameters exhibited the highest values in the loading matrix relative to PC2. Samples subjected to pre-cooking and freeze drying exhibited distinct clustering in PC2. This indicates a technological and functional quality axis that is strongly associated with pigment retention, visual attributes, mineral content, and antioxidant capacity. The clustering of carotenoids, chroma, and L* values suggests that color preservation was associated with pigment stability, especially in the freeze-dried samples. Additionally, the correlation of DPPH scavenging activity and FRAP values with carotenoids and minerals indicates that the antioxidant activity was not only related to phenolic compounds but also to carotenoids and minerals.
The samples in the FTCOZL group exhibited the highest antioxidant potential (DPPH scavenging activity and FRAP values) and carotenoid levels. Additionally, the samples exhibited in the FTCOZL group exhibited the highest mineral content (Ca, Mn, Na, Fe, K, and Cu), with Mn exhibiting the strongest correlation. These findings suggest that pre-cooking, followed by freeze drying, is the most suitable processing condition for developing functional food ingredients with enhanced antioxidant potential, pigment retention, and mineral density. These powdered ingredients can be incorporated into nutritionally enriched food products, in which both technological performance and functional value are desirable.
Some nutritional and bioactive compounds may be lost during the freeze-drying process. However, the performance of this dehydration method in preserving nutritional quality, especially when performed under vacuum, is superior to that of other techniques. Furthermore, the quality parameters, such as rehydration capacity and porosity, of freeze-dried food products are suitable for various food applications, including the production of beverages, soups, and baked goods (Bhatta, Stevanovic Janezic & Ratti, 2020). PCA revealed the technological relevance of freeze drying, especially when combined with cooking. Pre-cooking, followed by freeze drying, can be a potential strategy to optimize the functional and nutritional qualities of taioba leaves for food applications.
Phenolic compounds
Table 4 presents the phenolic compounds identified in powdered taioba leaves, while Figure 2 illustrates their molecular structures.
Gentisic acid and catechin were not detected in FTCOZL, FTCOZD, and FTCRD samples. This indicates that gentisic acid and catechin are thermally unstable. Processing conditions involving heat exposure may adversely affect the stability of phenolic compounds, especially flavonoids, such as catechin, which are susceptible to oxidation and structural degradation during thermal treatment. (Wang et al., 2023) examined the effects of heat treatment on five catechin-based solutions (prepared with boiling water, heated for 180 min, and analyzed using HPLC). Catechin underwent decomposition with increasing heat exposure. This degradation was attributed to hydroxylation, dehydroxylation, and oxidation reactions during heating. The absence of catechin in most processed samples in this study is consistent with this behavior, highlighting the sensitivity of this compound to both thermal treatment and prolonged drying processes.
Moura et al. analyzed the phenolic acid and flavonoid profiles of taioba leaves (X. sagittifolium) and identified 11 compounds, including syringic acid (Moura et al., 2021). The authors also identified several hydroxycinnamic acids, which resemble compounds identified in taioba leaves in this study.
Studies on the optimization of the extraction of polyphenols from unconventional edible plants have reported that the caffeic acid content is the highest in lemongrass (366.78 ± 14.77 μg/g) and the lowest in chicory (245.67 ± 21.55 μg/g). Additionally, protocatechuic acid (63.14 ± 3.58 μg/g) was identified in ryegrass (Kiani et al., 2023).
The identification of thermally stable compounds, such as protocatechuic, caffeic, and coumaric acids, in all treatment groups suggests that powdered taioba leaves may represent a potential functional ingredient for developing food formulations requiring processing stability, including dehydrated soups, instant mixes, baked products, and powdered plant-based ingredients. In addition to the antioxidant potential, the persistence of these phenolics after drying reinforces the technological potential of taioba as a natural source of functional compounds for nutritionally enriched food systems.
Volatile compounds
The quantification of volatile compounds in freeze-dried raw and cooked taioba leaves is shown in Table 5, while that in oven-dried raw and cooked leaves is shown in Table 6.
The detection of volatile compounds released by plants under different conditions during their development can provide useful insights into physiological processes and potential mechanisms (Harren & Cristescu, 2013). Cutting, wounding, and drying of leaves alter the composition and intensity of volatile organic compound release. These compounds are generally released in response to stress. For example, leaf damage promotes the oxidative cleavage of membrane fatty acids (such as linoleic and α-linolenic acids), inducing the release of aldehydes and alcohols, including C6 compounds (six-carbon molecules), such as members of the hexanal and hexenal families (Fall et al., 1999). In FTCOZD samples, (E)-2-hexenal was detected in small amounts. These findings are consistent with the physiological response of the plant, which rapidly produces hexanal and hexanal compounds in response to wounding. Hexenal and hexanal compounds exhibit antibiotic properties, inhibiting the microbial invasion of damaged tissues (Croft, Juttner & Slusarenko, 1993). The release of hexanal and hexenal compounds further potentiates the antibiotic properties. For example, (Z)-3-hexenal serves as a precursor in the degradation process (Brilli et al., 2011).
During drying, volatile emission is accelerated due to the reduction in water content, which leads to cellular collapse and promotes the formation of volatiles (Bamberger et al., 2010). In the freeze-dried samples, alcohols were the predominant volatiles, followed by ketones. This suggests the preservation of fruity and herbaceous notes. In contrast, aldehydes and acids were the predominant volatiles in oven-dried samples, indicating enhanced lipid oxidation and amino acid degradation.
In all treatment groups, volatiles primarily belonged to alcohols, ethers, esters, alkanes, ketones, acids, and aldehydes (Tables 5 and 6). Alcohols were the predominant class in the freeze-dried samples.
In FTCRL samples, 14 volatile compounds were identified. Alcohols were the predominant volatile compounds, accounting for most of the peaks in the gas chromatography mass spectra. Cooking promoted the degradation of some compounds. Only 11 volatiles were detected in FTCOZL samples, with alcohols being the predominant group. Some compounds, such as dodecane and ethanol, exhibited two peaks, corresponding to monomeric and dimeric forms. The high proton affinity of dodecane and ethanol may explain dimer formation as ions migrate through the drift tube after chromatographic separation (Pan et al., 2022).
The FTCRD and FTCOZD samples comprised 15 and 13 volatile components, respectively. Aldehydes were the predominant volatile compounds, followed by alcohols. Unique compounds belonging to terpenes and lactones were also detected in FTCOZD samples.
Several compounds of sensory relevance associated with fruity notes were identified. Additionally, 1-pentanol associated with spicy aromas was detected (Xu et al., 2023; Yang et al., 2022). Diacetyl (2,3-butanedione) and acetoin, which were detected in oven-dried samples, contribute to buttery and creamy notes in fermented plant-based matrices (Rajendran, Silcock & Bremer, 2023). The occurrence of diacetyl (2,3-butanedione) and acetoin in taioba leaves can be attributed to thermally induced reactions rather than intrinsic plant characteristics.
Several compounds, including 1-penten-3-ol, 1-propene, 3-propoxy-, undecane, 2,3-pentanedione, acetoin, 5,9-undecadien-2-one, 6,10-dimethyl-(Z)-, 2,3,4-trimethyl-hex-3-enal, and cyclopentasiloxane, decamethyl-, underwent degradation in samples subjected to cooking, followed by freeze drying. The aromatic compound 1-penten-3-ol is reported to be upregulated in certain foods, such as teas (Camellia sinensis), red tea, and herbal teas, but downregulated in black tea, kohlrabi (Brassica oleracea var. gongylodes), and green tea. However, 1-penten-3-ol has not been quantified in legumes and asparagus (Asparagus officinalis).
Freeze drying preserves the contents of alcohols and ketones, which tend to undergo thermal degradation. In contrast, oven drying preserved the contents of aldehydes and volatile acids, especially in the cooked samples, which can be attributed to lipid oxidation and amino acid degradation. Pre-cooking promoted the formation of certain volatiles, such as 2-methylbutanal, especially in FTCOZD samples. This suggests that cooking with moist heat, followed by oven drying, accelerates degradation reactions, altering the aromatic profile.
Thus, freeze drying preserves sensory volatile compounds (alcohols and fruity/herbaceous ketones), whereas oven drying enhances compounds derived through oxidation and thermal degradation (aldehydes, acids, and esters). These differences have direct technological implications. In particular, freeze-dried products may be suitable for innovation targeting sensory and functional properties, while oven-dried products may be suitable for developing products with intense aromatic profiles.
Conclusions
Powdered taioba leaves exhibited high nutritional value and antioxidant potential. This study, for the first time, reported the volatile profile of X. taioba, revealing the functional and technological relevance of this species. Processing methods, especially freeze drying, influenced the preservation of phenolic compounds, antioxidant activity, pigments, and aromatic compounds in taioba leaves. Thus, taioba is a potential functional ingredient for developing plant-based food products. However, further studies are warranted for the bioaccessibility and sensory acceptance to enable their industrial application.
Data Availability Statement
Data available upon request to authors.
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Editor de seção:
Renato Paivahttp://orcid.org/0000-0001-5107-0285
