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Article • Quím. Nova 49 • 2026 • https://doi.org/10.21577/0100-4042.20260067 linkcopy

Open-access OPTIMIZATION OF THE EXTRACTION OF VOLATILE COMPOUNDS FROM THE PULP OF THE “SABOROSA” FRUIT (SELENICEREUS SETACEUS)

AuthorshipSCIMAGO INSTITUTIONS RANKINGS

Abstract

“Saborosa” (Selenicereus setaceus) is a fruit native to the Brazilian Cerrado that remains poorly studied regarding its volatile organic compound (VOC) profile. This study aimed to optimize VOC extraction from the pulp using headspace solid-phase microextraction and gas chromatography-mass spectrometry (HS-SPME/GC-MS) and three semipolar fibers (polydimethylsiloxane/divinylbenzene (PDMS/DVB), carboxen (CAR)/PDMS/DVB, and CAR/PDMS) under different extraction times and temperatures. A total of 24 compounds were identified, including organic acids, ketones, alcohols, esters, hydrocarbons, monoterpenes, and sesquiterpenes, with 20 compounds reported for the first time in this species. Extraction time significantly influenced the performance of the CAR/PDMS/DVB fiber, whereas temperature affected PDMS/DVB, resulting in higher compound recovery. The CAR/PDMS fiber showed no significant dependence on these variables. Optimal extraction conditions were 35 °C and 60 min, yielding the highest number of analytes. The identified VOCs contribute to key sensory and identity descriptors of the fruit. Compounds such as hexanal, 1-hexanol, 3-methylbutan-1-ol, and (E)-2-octenal were associated with fruity and citrus-green notes. These results expand the chemical knowledge of this still underexplored species and may be associated with fruit quality markers. To date, this is the most comprehensive and optimized study on VOC extraction and characterization from S. setaceus pulp.

Keywords:
Cactaceae; dragon fruit; GC/MS; HS-SPME; Brazilian savanna.

INTRODUCTION

The Cerrado is recognized as the tropical savanna with the greatest biological diversity in the world and is the second-largest biome in South America. It occupies approximately 22% of Brazilian territory and is notable for its wide variety of climates, soil types, and highly diverse fauna.1 The vegetation of the Cerrado also deserves attention: it comprises more than 6,000 plant species, many of which exhibit unique forms, vibrant colors, exotic flavors, and significant potential for agricultural and technological applications.2,3Among these plants, native fruits stand out for their distinct nutritional properties, diverse sensory attributes, and bioactive compounds that promote health.4

The Cerrado pitaya (Selenicereus setaceus), commonly known in Brazil as “saborosa”, mini pitaya, or baby pitaya, is a cactus that remains commercially underexplored and is largely unknown to the general population. The fruit has white pulp with numerous edible seeds, is sweet and juicy, and exhibits unique and pleasant sensory characteristics suitable for fresh consumption. Additionally, it can be used in the production of ice creams, jams, juices, and in the development of various other yet-unexplored products.5-7

Compared to other commercially widespread fruit-bearing cacti, such as Selenicereus undatus (purple skin with white pulp) and Hylocereus polyrhizus (purple skin with red pulp), which are originally native to southern Mexico, the Pacific regions of Guatemala, Costa Rica, and El Salvador, the Cerrado pitaya still faces resistance to large-scale commercial exploitation. Its cultivation is largely limited to cactus collectors, or it grows spontaneously in nature through seed dispersal by predators.5,7,8 From a sensory perspective, the Cerrado pitaya stands out for its sweeter taste compared to other commercially known pitayas, such as those with white or red pulp. Being a smaller fruit than Selenicereus undatus, Hylocereus polyrhizus, and their cultivated hybrids worldwide, the Cerrado pitaya has a higher concentration of soluble solids, as well as more intense flavor and aroma.8

Aroma, as well as taste, is essential for the acceptance of food products and is a sensory aspect that greatly influences the selection of these fruits. The presence of sugars, organic acids, and other compounds directly affects the flavor of the fruit, whereas the aroma involves a variety of volatile substances, such as ketones, lactones, aldehydes, hydrocarbons, alcohols, and acids.9,10 The presence of these volatile compounds in the fruits indicates an intense and distinctive aromatic identity, common to Cerrado fruits.11,12 According to Wu et al.,9 volatile compounds are important indicators of fruit quality and flavor, and together with aroma, they are directly related to the sensory acceptance of products. These compounds also contribute to the ability of the fruit to withstand external stresses.13

Solid-phase microextraction (SPME) is recognized as a green method for extracting volatile and semi-volatile compounds, that is, without the use of organic solvents. The compounds can be extracted using different coating layers and released from the fiber in the hot injector of the gas chromatograph (GC) through the phenomenon of thermal desorption, enabling their subsequent analysis.14 Therefore, it is important that these analytes have affinity for the fiber used, which may have different properties and thicknesses.

The fiber coating is crucial for the quantity of compounds extracted from the sample.15 Physically, the polydimethylsiloxane (PDMS) fiber is nonpolar, whereas polyacrylate and carboxen (CAR), and divinylbenzene (DVB) fibers are considered polar. The use of mixed coatings, such as PDMS/DVB, CAR/PDMS, and DVB/CAR/PDMS fibers, increases extraction efficiency by enhancing the retention of compounds with varying polarities and volatilities.15 In mixed coatings, adsorption and absorption mechanisms are the combined properties that enable the extraction of analytes.16 Thus, different compounds can be identified depending on the coating thickness and the polarity of the fibers used.17

In this context, given that the Cerrado pitaya is a scarcely studied fruit with limited information available in the scientific literature, particularly regarding its chemical composition, the aim of this study was to optimize the extraction conditions for volatile organic compounds from the fruit pulp. This was achieved by employing three different mixed-coating fibers - DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS - under varying temperatures and exposure times.

EXPERIMENTAL

Sample preparation

The Cerrado pitaya (Selenicereus setaceus) was collected in the rural area of Conceição do Castelo, Espírito Santo, Brazil (20°17’44” S, 41°15’29” W). A total of 5 kg of fruits were harvested manually using pruning shears, randomly and from the same plants. The fruits were collected intact, with the skin showing the typical pink coloration and a soft texture when gently pressed. The total soluble solids content (°Brix) was measured using a refractometer, showing values of 14% in the pulp of the “saborosa”, close to those reported in the literature,6 indicating its optimal ripeness for harvesting and consumption. The fruits were washed under running water to remove surface impurities. Subsequently, the pulp and peel were manually separated, portioned, and stored in laminated bags at -18 °C until further analysis.

Extraction of volatile organic compounds (VOCs)

The determination of VOCs in the seedless pulp of the pitaya followed the methodology proposed by Mariano et al.12 To promote greater volatility of the analytes, 0.175 g of NaCl was added to 0.5 g of pulp, which had been previously placed in glass vials with a 20 mL headspace and sealed with screw caps and rubber septa. The headspace solid-phase microextraction (HS-SPME) method was used for the extraction and identification of VOCs.

Experimental design

The optimal extraction conditions were determined using a 22 factorial design with triplicate at the central point, as described in Table 1. The number of volatile compounds detected was used as the response for the variables studied.

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Table 1
Variables used in the 22 factorial design with triplicate at the central point for the optimization of HS-SPME conditions

The experimental design was used to evaluate three types of fibers: DVB/CAR/PDMS (50/30 μm), PDMS/DVB (65 μm), and CAR/PDMS (85 μm), all obtained from Supelco®. For this purpose, a heating plate and an aluminum block equipped with a thermometer were set up so that the SPME device containing the fiber could be adequately exposed to the vials. After extraction, the fibers were retracted and immediately inserted into the GC MS for compound desorption.

Experimental conditions

The volatile compounds were analyzed using a gas chromatograph coupled to a mass spectrometer (GC-MS QP2010 Plus, Shimadzu Corporation, Japan). All fibers used were conditioned in the chromatograph according to the recommendations of the manufacturer for each fiber type.

A 5-min preheating step was applied to the vials containing the samples at the designated temperature for each treatment to determine optimal conditions for achieving partition equilibrium between the analytes and the fiber in the headspace mode, resulting in greater recovery of volatile organic compounds after chromatographic analysis. After preheating, the fibers were exposed to the proposed times and temperatures for analyte adsorption. After the extraction period, the fibers were inserted into the chromatograph injector at 270 °C for 5 min to allow desorption of the extracted VOCs.11

The compounds were separated using an HP-5 MS capillary column (5% phenyl and 95% methylpolysiloxane, Agilent Technologies Inc., Germany) with a length of 30 m, an internal diameter of 0.25 mm, a film thickness of 0.25 μm, and helium as the carrier gas at a constant flow rate of 34.8 mL min-1. The injector (split mode 5:1) was maintained at 270 °C for 5 min. The oven was programmed to 40 °C for 1 min, followed by a ramp rate of 3 °C min-1 to 140 °C, held for 2 min. The temperature was then increased at 10 °C min-1 up to 180 °C, and finally at 30 °C min-1 up to 245 °C, where it was held for 1 min.

Data acquisition was performed in full-scan mode using electron impact (EI) ionization at 70 eV, with a mass range of 29-600 m/z. The identification of volatile compounds was based on the mass to charge ratio (m/z) of the ionic fragments in the sample, using each mass spectrum within the range of 50 to 300 m/z. The peaks observed in the chromatograms were tentatively identified using data obtained from the NIST 11 (National Institute of Standards and Technology, USA, 2011) library, considering a similarity index above 80%. This identification was also supported by articles7,13,18,19 reporting volatile compounds in cactus fruits. The total peak area was obtained using the GC-MS Solution software, version 4.20 (Shimadzu Corporation, Japan) and analyzed in Microsoft Office Excel 2010 (Microsoft Corporation, USA).

RESULTS AND DISCUSSION

To determine the optimal extraction conditions for volatile organic compounds using HS-SPME, the effects of temperature and exposure time for each fiber were evaluated. The DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS fibers were analyzed and compared individually according to the total number of identified compounds.

Using the three fibers, a total of 24 volatile constituents were identified in the pulp of “saborosa” fruit (Table 2). These volatile components were categorized as organic acids (12.5%), ketones (8.33%), aldehydes (16.66%), alcohols (20.83%), esters (20.83%), hydrocarbons (12.5%), monoterpenes (4.16%), and sesquiterpenes (4.16%).

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Table 2
Volatile profile of “saborosa” fruit extracted using different fibers

When evaluating the fibers individually, it was observed that the PDMS/DVB fiber adsorbed 16 compounds, followed by DVB/CAR/PDMS with 14 compounds, and finally CAR/PDMS, which showed the lowest adsorption, with 8 compounds. When assessing the major chemical classes extracted, the PDMS/DVB fiber proved to be more efficient at extracting aldehydes, while the DVB/CAR/PDMS fiber proved to be more efficient at extracting alcohols. Both fibers were equally efficient at extracting esters. The CAR/PDMS fiber did not show a strong signal for any chemical class.

Coating combinations such as DVB and CAR can influence the porosity and polarity of the fiber, potentially improving analyte retention. The synergistic effects of both adsorption and absorption in the stationary phase of the PDMS/DVB and DVB/CAR/PDMS fibers suggest a higher analyte retention capacity compared to the CAR/PDMS fiber.30 Due to its characteristics, the CAR/PDMS fiber shows better performance in the extraction of highly volatile compounds, associated with its porous solid coating, suggesting higher extraction through adsorption.31

In the evaluation of organic compounds present in the pulp of Selenicereus setaceus using the PDMS/DVB fiber,7 it was observed that among the 12 identified compounds, esters were the most abundant, representing 50% of the total, 33.3% were aldehydes, and 17.7% were alcohols. According to the authors,7 the esters identified in “saborosa” pulp increase as fruit ripens.

Obenland et al.18 evaluated the presence of volatile compounds in six pitaya fruit varieties from the species H. undatus, H. costaricensis, and H. polyrhizus, identifying a total of 34 aroma volatiles using the CAR/PDMS fiber, with aldehydes being the most abundant (90%).

In the white-fleshed pitaya,10 a total of 60 VOCs were detected in different cultivars using the DVB/CAR/PDMS fiber, with the headspace vials incubated at 60 °C for 10 min. Most of the identified compounds belonged to the aldehyde, ester, alcohol, and alkane classes. According to the authors,10 n-hexane, 1,3-dioxol-2-one, pentadecane, ethyl octanoate, benzeneacetaldehyde, hexanal, and 1-hexanol were the main compounds identified in the fruit pulp.

The evaluation of three cultivars of Opuntia ficus-indica cactus fruits revealed the presence of 40 volatile constituents, with aldehydes and ketones being the most represented compounds, accounting for 32.4 and 27.6%, respectively.32 The authors used the DVB/CAR/PDMS fiber for the adsorption of the compounds under extraction conditions of 30 min at 50 °C.

Tomas et al.,7 also reported the presence of alcohols in the pulp of “saborosa” from the Cerrado, such as 1-hexanol and 1-pentanol, and concluded that these compounds increase their relative area as the fruits mature. This increase is related to fruit senescence. Sensory-wise, alcohols play important roles; for example, 1-pentanol has been identified in Hylocereus polyrhizus pitaya and is associated with the sweet balsam descriptor.22 Compounds such as hexanal, 1-hexanol, and 3-methylbutan-1-ol are associated with the fruity descriptor.22 In addition, hydrocarbons such as dodecane and tridecane, also reported by Santos et al.,22 were associated with the alkane sensory descriptor. For the first time in the literature, the compounds allyl acetate and caryophyllene have been reported for a cactus fruit; however, their sensory information still remains limited. The different fibers were also evaluated for their extraction efficiency, as well as for the effects of exposure time and temperature on the recovery of volatile organic compounds (Figure 1).

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Figure 1
Effects of parameters: time and temperature on volatile extraction using different fibers for HS-SPME: DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS

From the Pareto chart, generated based on the number of compounds, it is possible to observe that for the two evaluated parameters, there was no significant difference when using the CAR/PDMS fiber. For the DVB/CAR/PDMS fiber, however, the increase in temperature was the significant variable for the greater adsorption of the number of compounds. In contrast, for the PDMS/DVB fiber, the presence of a greater number of analytes increased with time.

The surface graphs (Figure 2) show the influence of time and temperature on the extraction of the number of volatile compounds using the different fibers evaluated.

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Figure 2
Three-dimensional response surface (RSM) plots of extraction time and temperature parameters in the extraction of volatile compounds using different fibers for HS-SPME: DVB/CAR/PDMS, PDMS/DVB and CAR/PDMS

The evaluation of the response surface plots for the DVB/CAR/PDMS fiber confirms the influence of temperature on analyte adsorption, with higher temperatures resulting in a greater number of compounds obtained. For the PDMS/DVB fiber, it is observed that the longer the exposure time of the fibers, the greater the number of analytes obtained. For the CAR/PDMS fiber, the model is not significant for any of the variables studied.

Figure 3 shows the chromatograms obtained under the best time (35 min) and temperature (60 °C) conditions for each fiber used, highlighting the individually identified compounds and their chemical structures for each type of coating used in adsorption.

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Figure 3
Chromatograms generated for sapodilla pulp of volatile compounds extracted with the DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS fibers

Thus, it was observed that the DVB/CAR/PDMS and PDMS/DVB fibers were more efficient at extracting a greater number of compounds from different chemical classes. Both are considered mixed coatings and are effective at extracting compounds of different polarities. A temperature of 35 °C and an exposure time of 60 min were the conditions that yielded the highest number of compounds extracted for both fibers. To date, no study in the literature has investigated the best conditions for extracting volatile organic compounds from the pulp of the Cerrado “saborosa” using different fibers, times, and exposure temperatures.

CONCLUSIONS

The pulp of the “saborosa” is composed of a complex mixture of volatile compounds, most of which belong to alcohols, esters, aldehydes, hydrocarbons and organic acids. The DVB/CAR/PDMS and PDMS/DVB fibers were the most efficient and similar in extracting a greater number of analytes compared to CAR/PDMS. This study identified volatile compounds in the fruit pulp that have not yet been described in the literature. In general, the study of these analytes allows for the understanding of the main chemical components of the pulp and helps in understanding sensory characteristics such as flavor and aroma in cactus fruits. It also provides valuable information for future studies involving better conditions and treatments that increase the shelf life of the “saborosa” without decreasing its acceptance by consumers and its sensory quality aspects. Finally, this study contributes to a better understanding of the unprecedented chemical composition of a little-known Brazilian Cerrado fruit, the “saborosa”.

ACKNOWLEDGMENTS

This work was supported by CAPES (code 001), CNPq (132217/2023-6, 307787/2022-2, 404432/2024-7), GEPEQF, and FAPEMIG (APQ-04336-23, BPD-00858-22, 5.308/15). The authors also acknowledge UFSJ, UFMG, CAPES, CNPq, FAPEMIG, the LEAF unit (ISA, Lisbon, Portugal), and GEPEQF.

DATA AVAILABILITY STATEMENT

All data generated or analyzed during this study are included in this published article.

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Edited by

  • Associate Editor handled this article:
    Fernanda G. Finelli

Publication Dates

  • Publication in this collection
    26 June 2026
  • Date of issue
    2026

History

  • Received
    15 Feb 2026
  • Accepted
    27 Mar 2026
  • Published
    06 May 2026
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