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Article

Thermal Properties of Ultrasound-Extracted Okra Mucilage

1
Food Processing Department, Efes Vocational School, Dokuz Eylül University, İzmir 35920, Turkey
2
Food Engineering Department, Engineering Faculty, Ege University, İzmir 35100, Turkey
*
Author to whom correspondence should be addressed.
Appl. Sci. 2023, 13(11), 6762; https://doi.org/10.3390/app13116762
Submission received: 2 May 2023 / Revised: 27 May 2023 / Accepted: 31 May 2023 / Published: 2 June 2023
(This article belongs to the Section Food Science and Technology)

Abstract

:
Utilizing chemical and physicochemical techniques, the mucilage part of okra was extracted with the use of ultrasound, and the polysaccharide extract’s structural and thermal characteristics were assessed. Analysis of the extraction yield revealed that there was no discernible impact of time and that the yield increased with a decreasing okra to distilled water ratio (mean 8%). Differential scanning calorimetry was employed to determine the phase change enthalpy by examining the glass transition temperature and enthalpy. The glass transition temperatures of the samples were found to be about 50 °C and the melting temperatures were in the range of 166–170 °C for varied solid/solvent ratios (1:10, 1:25, 1:30, and 1:50) and extraction durations of 5 and 30 min. Using thermogravimetry (TG) and differential thermogravimetry (DTG) techniques, it was discovered that the okra polysaccharides were thermally stable with considerable weight loss above 240 °C. For the purpose of illuminating the bonds of the polysaccharides, FTIR analysis was used to characterize the polysaccharides obtained by the varying extraction times and rates of solid/solvent. This analysis provides detailed information about the composition of the extracts. It was found that the molecular structure of the mucilage from okra was unaffected by the varying ratios and times. The study’s findings indicated that the use of ultrasound could be a promising approach for extracting polysaccharides that possess strong thermal stability, making them suitable for use in various industrial applications. The study noted that variations in ultrasound application time and solid/solvent ratios did not appear to impact the thermal stability of the extracted polysaccharides. The important parameters for the extraction conditions such as the time and low amount of sample used are preferred for applications. The findings obtained indicate that ultrasonic extraction application at a 1/50 solid/solvent ratio for 5 min is statistically significant in terms of thermal properties and yield. These findings could have important implications for the energy costs associated with the industrial use of ultrasound extraction.

1. Introduction

Currently, many micro- and macro-components that can be extracted from plants are of great interest to different consumer demands. Among these components, polysaccharides are of great interest because of their biological and pharmacological properties, including antitumor, antiviral, antioxidant, and anti-inflammatory activities. Okra (Abelmoschus esculentus) referred to as lady’s finger is considered both a vegetable and a medicinal crop and is typically grown in tropical, subtropical, and temperate regions around the globe; it is a flowering plant that is widely cultivated and consumed as a vegetable in many parts of the world [1]. Okra is a flowering plant that belongs to the mallow family. Unripe and tender fruits are consumed as vegetables. Okra is rich in protein, fat, carbohydrates, calcium, phosphorus, iron, and numerous vitamins, all of which provide numerous health benefits such as reducing fatigue and quickly restoring physical strength. Okra has various applications in the food, pharmaceutical, and biomedical sectors. Okra mucilage is a thick liquid extracted from okra pods that contains random coil polysaccharides, such as galactose, rhamnose, and galacturonic acid [2,3,4,5].
Currently, studies are being carried out on the development of different extraction methods because of the time-consuming nature and limited efficiency of classical extraction methods. Various techniques, including hot water extraction, enzyme-assisted extraction, microwave-assisted extraction, ultrasound-assisted extraction, and subcritical water extraction, are commonly employed for the extraction of bioactive polysaccharides from okra [6,7,8]. One of the extraction methods that has been studied and used in the last few decades is ultrasound-assisted extraction. The utilization of ultrasonic-assisted extraction (UAE) is a popular, non-thermal technique that is employed to extract bioactive polysaccharides from a diverse range of sources, such as okra polysaccharides, seaweed-derived alginates and carrageenans, and brewer’s-yeast-derived β-glucan. UAE operates by utilizing mechanical, thermal, and cavitation phenomena [6,9,10,11]. Ultrasound-assisted extraction is the simplest and most versatile method for cell disruption and extraction. With this method, it is possible to increase the extraction efficiency and yield and shorten the extraction time by exposing the material to ultrasonic sound waves. It has been shown to have a number of beneficial effects, including making the product lighter, improving its emulsifying properties, antioxidant activity, and reducing impurities [12].
The thermal properties of food include the specific heat and enthalpy, thermal conductivity, diffusivity, and heat penetration coefficient. Knowledge of the thermal properties, such as the specific heat and thermal conductivity, is necessary for effective thermal design [13]. Heat conduction is the predominant type of heat transfer that occurs during the processing and storage of food and agricultural products. According to reports, the preliminary structural characteristics and thermal stability of bioactive polysaccharides extracted utilizing a variety of extraction procedures remained mostly unaltered [6,14].
In this study, the mucilage part of okra vegetables, which has an important role in terms of food and health, was obtained by ultrasound-assisted extraction, which is an environmentally friendly and economical extraction method, and the structural and thermal properties of this polysaccharide extract were determined by chemical and physicochemical methods. One of the important objectives of our study is to determine the effects of ultrasound extraction technology at different solid/solvent ratios and times on the thermal stability and molecular characterization of the products. The utilitarian goal of obtaining and characterizing the mucilage of okra under different extraction conditions and determining its thermal properties could be to explore and utilize the mucilage for various practical applications. These polysaccharides can be widely used in the food industry as thickeners because of their sticky and gamy structure, viscosifiers, gelling agents, and emulsifiers [9,15]. This research can lead to the development of innovative and sustainable products that utilize the unique properties of okra mucilage.

2. Materials and Methods

2.1. Materials

Polysaccharides were extracted from fresh and dried okra samples. Fresh okra pods (Abelmoschus esculentus), approximately 3 cm in diameter and 7 cm in length, were purchased from a local market in Izmir, Turkey. The season for okra in Turkey is from mid-June to the end of summer. A solar dryer (Tartes Tarim, Izmir, Turkey) was used to obtain the dried okra. The dried okra was ground to a 400–500 µm powder using a hammer mill (Brook Crompton Controls, Wakefield, UK) and stored under suitable storage conditions.
The ethanol (96% extra pure) used for polysaccharide purification was purchased from Tekkim Kimya (Bursa, Turkey).

2.2. Methods

2.2.1. Ultrasound-Assisted Extraction Method

The steps used in the ultrasound-assisted extraction of polysaccharides from okra (UAEOP) are shown in Figure 1c. Ground and powdered okra were prepared by adding distilled water in different ratios (1:10, 1:25, 1:30, and 1:50 g/mL). Ultrasonic-assisted extraction was performed using a high-intensity probe system ultrasonic device (Hielscher UP400S, 24 kHz, Germany) equipped with an H14 probe (14 mm diameter; 90 mm height) at an initial temperature of approximately 10 °C in a double-walled glass sample container of 250 mL volume and 150 mL sample volume, with the probe placed in the center of the sample. The energy consumed by the ultrasound set-up (the ultrasound power) was recorded instantaneously using a wattmeter (Voltcraft Energy Check 3000; Germany). A water bath was used for temperature control, and the extraction process was performed at 200 W for 5, 10, 15, and 30 min (Figure 1a).
The extract was centrifuged (Hettich Universal 320R, UK) at 2000× g for 15 min. The separated supernatant fractions were combined and filtered through a fine-mesh cheesecloth and concentrated in an evaporator at 70 °C at a rotation speed of 100 rpm to approximately 1/3–1/4 of the initial volume. The concentrated polysaccharide-containing solution was precipitated and purified by adding approximately six times its volume of ethanol and then centrifuged at 5000 g for 10 min to remove impurities. For preservation, the samples were freeze-dried and stored at 20 °C. Photographs of the fresh and freeze-dried okra polysaccharides are shown below (Figure 1b).

2.2.2. Ultrasound-Assisted Extraction Yield

The extraction yields were calculated by proportioning the mass of okra powder to the mass of dried okra powder (dry basis) using Equation (1) [16] as follows:
Yield (%) (w/w) = (okra powder(g)/Initial okra mass(g)) × 100

2.2.3. Fourier Transform Infrared Spectroscopy (FTIR)

Fourier transform infrared spectroscopy (FTIR) analyses of the UAEOP were performed at 400 to 4000 cm−1 wavelengths and room temperature using a Thermo Scientific NICOLET iS10 (Thermo Fisher Scientific, Waltham, MA, USA) device [17].

2.2.4. Thermal Characterization

Differential Scanning Calorimetry (DSC)

DSC (Q100, TA Instruments Inc., New Castle, DE, USA) was used to determine the thermal properties of the UAEOP. Hermetic aluminum pans were used to cover the samples (five mg) and heated at a rate of 5 °C/min from 20 to 200 °C to determine the melting enthalpy, melting onset temperature, and melting point and from 10 to 100 °C to determine the glass transition temperature. An appropriate amount of distilled water was then added to the reference cells. Nitrogen was used as the carrier gas at a flow rate of 50 mL/min. The data were analyzed using TA Universal Analysis software (https://www.tainstruments.com/support/software-downloads-support/downloads/, accessed on 26 May 2023).

Thermogravimetric Analysis (TGA)

A thermogravimetric analyzer (TGA SDT Q600, TA Instruments, New Castle, DE USA) with a regular flow of nitrogen provided at a rate of 100 mL/min was employed to determine the thermal stability of 7 mg of the UAEOP in a temperature range varying between 20 °C and 1000 °C at a rate of 10 °C/min. Within the heating range, the weight loss rates due to the thermal decomposition were calculated by a comparison of the original weight with the data of weight loss [18].

2.2.5. Statistical Analysis

All experiments were repeated three times, and the data were expressed as means ± standard deviations. The data were analyzed using SPSS software V20 (IBM, Armonk, NY, USA). Statistical significance was determined by one-way ANOVA, taking a level of p < 0.05 as significant to Tukey’s range test. For the yield analyses, differences within the same groups were determined by an independent t-test.

3. Results and Discussion

3.1. Yield of the Ultrasound-Assisted Extraction of Okra Polysaccharides (UAEOP)

The yield (%) values calculated for the extracts obtained using different solid-to-solvent ratios and by applying different extraction times are shown in Table 1.
The highest yield was found at a solid/liquid ratio of 1:50 (p < 0.05). The yield increased as the okra/distilled water ratio decreased, but time had no significant effect on the yield (p > 0.05). At 1:10 and 1:25 solid/liquid ratios, it can be seen that the yield decreased as time increased (p < 0.05). Because the 1:10 and the 1:25 consistencies are very dense, the ultrasound could not work for long, and the temperatures increased excessively. Zhai et al. [4] reported a yield of 6.37% in their study investigating the effects of different temperatures on the yield of ultrasound-assisted extraction of polysaccharides from okra. Similarly, our study suggests that as the okra density increases, ultrasound-induced molecular vibrations may be accelerated, leading to an increase in temperature. According to Zhao et al. [19], the yield of asparagus increased over the extraction temperature range of 60 to 80 °C. On the other hand, unnecessarily prolonging the extraction time at a high temperature (80 °C) may cause polysaccharide breakdown and, as a result, reduce the yield of asparagus by 2.151 percent. When the bubbles collapsed as a result of the compression’s increase in both pressure and temperature, a powerful shock wave was created that cut through the solvent and improved the mass transfer through the entire system. Once the cell walls were breached, an ultrasonic wave passed through them and rinsed out the contents of the cells. In another study, Archana et al. [3] found a yield of 8.6% when testing different extraction techniques for okra polysaccharide extraction. Okra mucilage yields reported in the literature vary. Alvarenga Pinto Cotrim et al. [20] were reported to yield approximately 2.76 wt%. Kaur et al. [21] obtained about 0.5%.
By varying factors such as extraction time, temperature, number of cycles, and solvent/material ratio, many researchers have attempted to determine the most appropriate extraction conditions. The water-based extraction method employed by Lee et al. [22] resulted in a yield of 2.38% for the extraction of mucilage from okra. Samavati [23] utilized water exclusively as a solvent for the extraction of okra mucilage, which yielded a remarkably high percentage of 17%.
The variations in the values obtained could be attributed to several factors, including the region where the fruit is grown, the type of okra used, the portion of the okra plant utilized (i.e., calyx or pulp), the maturity stage of the fruit (fresh/ripe okra), and the physical state of the okra (dried powder or aqueous seed). Additionally, the choice of solvent employed may also have an impact on the percentage yield. When the studies in the literature are examined, it can be seen that they are in parallel with the results we found.

3.2. Molecular Characterization of the UAEOP

FTIR analyses were performed to characterize the polysaccharides obtained as a result of different solid/solvent ratios and extraction times, providing detailed information about the composition of the extracts and helping to elucidate the bonds contained in the polysaccharides.
Analysis of the FTIR spectra (Figure 2) showed that different extraction conditions did not have a significant effect on the chemical structure of the extracts. Yuan et al. [24] reported similar results to our own, in that they found that various extraction techniques used under different conditions did not have an impact on the structure of okra polysaccharides.
As shown in the spectrum, the main peaks are in the wavelengths 3853, 3744, 3314, 2972, 2901, 2114, 1719, 1604, 1406, 1249, 1042, and 888 cm1. The evaluation of the main peaks shows that there are C-OH, C-O-C, C-C, and C-H bonds in the extract, especially peaks 1249 and 1042 and the vibration at wavelength 888 cm−1. The bands can be described as corresponding as follows: a broad absorption band in the range of 3415–3276 cm−1 can be attributed to the distinctive stretching vibration of O-H bonds and hydrogen bonding of hydroxyl groups [25,26]. In the case of galactose and rhamnose, the spectral bands detected between 3000–2800 cm−1 can be attributed to the stretching vibrations of C-H bonds, which consist of CH, CH2, and CH3 groups [17,27]. The absorption bands between 1730 cm−1 and 1720 cm−1 correspond to the C=O stretching vibration of the esterified groups [25], while the absorption band observed at 1604 cm−1 can be attributed to the bending vibration of O-H bonds [26]. The band detected at 1420 cm−1 corresponds to the bending vibrations of C-H or O-H bonds [28]. On the other hand, the frequency observed at 1240 cm−1 can be attributed to the stretching vibrations of C-O bonds in complex polysaccharides [20]. The intense absorption band detected in the range of 1000–1200 cm−1 is thought to be associated with the stretching vibrations of C-O and C-C bonds and the bending vibrations of C-OH bonds in carbohydrates [29]. The spectral peak observed at around 850–820 cm−1 indicates the presence of sulfate groups [30]. The absence of the typical spectral bands at 1651 cm−1 and 1555 cm−1, which are associated with protein, suggests that the amount of protein present in the UAEOP is relatively low [24,25].

3.3. Characterization of Thermal Properties

3.3.1. Differential Scanning Calorimetry (DSC)

The data obtained from the analysis at different scanning speeds are presented in Table 2. The melting enthalpy, melting and initial temperatures, and glass transition temperatures obtained from the DSC thermograms are shown in Figure 3.
Differential scanning calorimetry was employed for the purpose of determining various properties such as glass transition temperature, enthalpy, and phase change enthalpies. The glass transition temperatures of the samples obtained by extraction at different solid/solvent ratios and extraction times showed ranges between 41.65 and 5.96 °C, while the melting temperatures were in the range of 166.74–172.67 °C with ΔH values between 158.2 and 225.6 j/g (Table 2).
As shown in Figure 3, there are two endothermic peaks. The presence of bound moisture in okra gum is a well-known fact, and the initial peaks observed at approximately 140 °C during the process are indicative of the evaporation of bound moisture present in the okra gum sample. The evaporation temperature of bound moisture in okra gum is typically higher than the boiling temperature of water due to the presence of ionic bonds between water molecules and the polysaccharide linkages in the gum. As a result, a greater amount of heat is required to break these bonds and release the bound moisture [31]. The appearance of secondary peaks in the thermal analysis of the okra gum samples indicates the melting of the crystalline phase within the gum.
The sample obtained using a solid/solvent ratio of 1/10 and an ultrasound duration of 5 min exhibited the highest melting temperature among all the samples tested. The statistical analysis revealed that there were significant differences in the melting temperatures of samples obtained using 1/10 and 1/25 solid/solvent ratios at a 5-min ultrasound duration. However, no significant differences were observed in the melting temperatures when the solid/solvent ratios were changed, and the ultrasound duration was increased to 10 min; therefore, increasing the ultrasound time did not make a significant difference in the melting temperature.
Although there was no significant variation in the ratios of solids to solvents when the extraction time was five minutes, there was a statistically significant increase in the glass transition temperatures when the time was extended to ten minutes. This suggests that the material’s thermal stability is enhanced by augmenting its viscous structure at higher temperatures. Thus, extending the extraction time might result in physical and chemical transformations in the food’s molecular structure. The relationship between the solid/liquid ratio and the glass transition temperature was noted to be time dependent. Specifically, as the solid/liquid concentration ratio decreases, the glass transition temperature tends to increase. The highest glass transition temperature (52.96 ± 1.37) was observed in the sample extracted for 10 min with a solid/liquid ratio of 1/50. A higher glass transition temperature has positive effects on the stiffness, hardness, and dimensional stability of the product, which is advantageous for determining processing conditions and end-use properties in the industry. Okra extract possesses an average 𝑇g value of 47 °C, which indicates that it exists in a glassy state at room temperature and is relatively stable, as it does not undergo any extrusive chemical action during experiments or storage. In order to preserve its quality and functionality, it is advisable to store okra in a dry environment at or below room temperature, thereby minimizing any chemical changes in its molecular structure [31].
The melting and glass transition temperatures we measured align with the values reported by Zaharuddin et al. [31] for okra gum, which were Tm = 180 °C and Tg = 60 °C. Furthermore, Dimopoulou et al. [32] reported a melting temperature of 152 °C, while Alvarenga Pinto Cotrim et al. [20] found it to be 167 °C.
Based on the analysis of enthalpy values, it was observed that the highest enthalpy value was recorded for the sample extracted using a 1/30 solid/solvent ratio for 5 min, while the lowest enthalpy value was recorded for the sample extracted using a 1/10 solid/solvent ratio for 10 min. Additionally, the statistical analysis revealed that time has a significant effect on enthalpy values. This suggests that the duration of ultrasound exposure can affect the thermal properties of the sample, and hence, it is an important factor to consider in the extraction and analysis of polysaccharides. In summary, the sample extracted using a 1/30 solid/solvent ratio for 5 min requires more energy to undergo a transition or change in state, such as melting, compared to the sample extracted using a 1/10 solid/solvent ratio for 10 min, due to its higher enthalpy value.

3.3.2. Thermogravimetric Analysis (TGA)

To ensure the suitability of materials for various applications, it is crucial to understand their thermal stability. By understanding the behavior of polysaccharides under different thermal conditions, it is possible to predict their performance in applications such as food processing, pharmaceuticals, and cosmetics, among others. Therefore, studying the thermal stability of polysaccharides is a critical step in their characterization and application development.
The thermogravimetry (TG) and differential thermogravimetry (DTG) methods were utilized to examine the thermal stability of okra polysaccharides. These techniques involve heating a sample with a controlled temperature increase over time and measuring the resulting change in weight. TGA curves can be generated by plotting mass or % mass versus time or temperature at the end of the measurement, while DTA curves are obtained by taking the first derivatives of the TGA results with respect to time or temperature. These curves provide information about the rate of mass change during heating and can be used to assess the thermal stability of the material.
The TG and DTG curves were utilized to analyze the disintegration patterns of okra polysaccharides at elevated temperatures in samples with a 1:10 to 1:50 solid/solvent ratio (Figure 4).
The thermal stability of okra polysaccharides can be analyzed by examining the TGA curves, which can be divided into two stages according to Table 3. In the first stage, a small weight loss occurs due to the desorption of hydrogen-bonded moisture from the polysaccharide structure. The second stage corresponds to the degradation of the polysaccharide, which results in significant weight loss above 240 °C. Drawing from these outcomes, one can conclude that okra polysaccharides exhibit good thermal resistance. This finding is consistent with previous studies conducted by other researchers, who have stated that the key phase of polysaccharide fractions’ degradation usually takes place within the range of 210 to 320 °C [20,33,34].
The TGA curves of the okra polysaccharides (Figure 4) did not exhibit significant weight loss up to 200 °C, indicating a high level of thermal stability. This finding is consistent with the results reported by Zaharuddin et al. [31]. Okra polysaccharides’ high thermal stability makes them a promising material for various industrial applications where thermal stability is a critical requirement. Additionally, the statement also highlights that okra polysaccharides have higher thermal stability compared to other biopolymers such as starch.
Rosa et al. [35] explored the thermal stability of okra fibers using thermogravimetric analysis since natural fibers’ low thermal stability is one of the primary constraints in their use in biocomposites. They discovered that the TG curve of okra fibers showed three stages of weight loss. The first weight-loss stage (8%) occurred between 30 and 110 °C, which was ascribed to the fibers’ water evaporation. The second weight-loss stage (16.1%) was observed in the temperature range of 220–310 °C and was linked to the thermal depolymerization of glycosidic bonds of hemicellulose, pectin, and cellulose. The third weight-loss stage (60.6%) was observed in the temperature range of 310–390 °C and was related to the disintegration of α-cellulose in the fiber. A residual weight percentage of 7.6% was found.
According to the authors, the outcomes of cellulose decomposition in an inert atmosphere comprised carbonaceous remains and potential non-reduced fillers. Overall, the study indicates that the thermal stability of okra fibers is relatively low, and their degradation occurs at high temperatures, which may limit their use in some high-temperature applications.
These discoveries suggest that okra polysaccharides may be utilized in generating biomaterials to serve various objectives, including improving oven stability in cakes, enhancing stability during freeze–thaw cycles, inhibiting crystal growth, encapsulation, and maintaining the stability of suspensions or emulsions in coloring agents. These applications can be in the food, pharmaceutical, and cosmetic industries, where thermal stability is often a critical requirement. The unique composition and structure of okra polysaccharides make them a viable alternative to other biopolymers that may not possess similar thermal stability [3].

4. Conclusions

The investigation involved acquiring okra mucilage through ultrasound-assisted extraction using various conditions, followed by assessing the chemical and physicochemical properties of the resulting polysaccharide extract, in order to determine its structural and thermal characteristics. The findings are advantageous in enhancing comprehension of the correlation between the structure and function of okra polysaccharides, and the use of the ultrasound-assisted extraction method has promising potential as a technique for extracting okra polysaccharides that are thermally stable, namely, they have the ability to maintain its properties and structure when exposed to high temperatures or varying levels of heat, which makes them suitable for industrial applications that require heat resistance. The application of the ultrasonic extraction method, utilizing different conditions, did not cause any molecular-level changes to the okra mucilage. When analyzing the extraction yields, it was discovered that reducing the ratio of okra to distilled water resulted in an increase in the extracted substance yield. However, the duration of the extraction process did not appear to have a significant effect on the yield. Thus, it has been shown that ultrasound-assisted extraction of polysaccharides from okra can be used in large-scale industrial applications with maximum efficiency with short-term extraction of low amounts of raw material, remaining thermally stable in heat applications and without changing its chemical structure.

Author Contributions

Conceptualization, Ş.Ö.G. and Ş.T.; methodology, Ş.Ö.G. and Ş.T.; validation, Ş.Ö.G., T.A. and Ş.T.; formal analysis, Ş.Ö.G.; investigation, Ş.Ö.G. and T.A.; resources, Ş.Ö.G. and Ş.T.; data curation, T.A.; writing—original draft preparation, Ş.Ö.G. and T.A.; writing—review and editing, Ş.Ö.G. and T.A.; visualization, Ş.Ö.G. and T.A.; supervision, Ş.T. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. (a) Ultrasound measurement set-up, (b) polysaccharides of okra, and (c) the UAEOP from the dried okra.
Figure 1. (a) Ultrasound measurement set-up, (b) polysaccharides of okra, and (c) the UAEOP from the dried okra.
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Figure 2. FTIR spectra of okra polysaccharides obtained under different ultrasound-assisted extraction conditions.
Figure 2. FTIR spectra of okra polysaccharides obtained under different ultrasound-assisted extraction conditions.
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Figure 3. DSC thermograms of okra polysaccharides obtained under different ultrasound-assisted extraction conditions.
Figure 3. DSC thermograms of okra polysaccharides obtained under different ultrasound-assisted extraction conditions.
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Figure 4. Thermogravimetric analysis (TGA) of the UAEOP obtained under different conditions ((a): 1:10 g/mL, (b): 1:25 g/mL, (c): 1:25 g/mL, and (d): 1:50 g/mL).
Figure 4. Thermogravimetric analysis (TGA) of the UAEOP obtained under different conditions ((a): 1:10 g/mL, (b): 1:25 g/mL, (c): 1:25 g/mL, and (d): 1:50 g/mL).
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Table 1. Yields of the UAEOP obtained under different conditions.
Table 1. Yields of the UAEOP obtained under different conditions.
Solid/Solvent RatioTime (min)Yield (%)
1:10 g/mL *55.33 ± 0.21 d
302.52 ± 0.13 D
1:25 g/mL *56.13 ± 0.36 c
308.15 ± 0.19 C
1:30 g/mL59.79 ± 0.22 b
309.02 ± 0.35 B
1:50 g/mL511.04 ± 0.32 a
3011.63 ± 0.68 A
a–d, A–D Means with the same letter in different groups in the same time interval are not statistically significantly different from each other. * Within the same groups, the effects of different times were significant.
Table 2. Initial temperature (T0), melting temperature (Tm), glass transition temperature (Tg), and enthalpy change (ΔH) of okra polysaccharides obtained under different UAEOP conditions *.
Table 2. Initial temperature (T0), melting temperature (Tm), glass transition temperature (Tg), and enthalpy change (ΔH) of okra polysaccharides obtained under different UAEOP conditions *.
UAEOP Time
5 min10 min
UAEOP Ratios1/101/251/301/501/101/251/301/50
ΔH (j/g) *185.4 ± 9.90 c†185 ± 3.89 c224.3 ± 1.20 a214.05 ± 3.89 b†158.20 ± 1.41 d†185 ± 3.25 c225.60 ± 3.11 a203.50 ± 7.07 b†
Tm (°C) *167.63 ± 4.36 b172.67 ± 1.02 a169.92 ± 1.17 ab170.26 ± 0.97 ab†167.75 ± 2.04 b170.29 ± 1.39 a170.99 ± 1.17 a166.74 ± 0.64 b†
T0 (°C) *166.42 ± 5.35 a169.12 ± 0.34 a†168.89 ± 0.80 a169.46 ± 0.54 a†165.40 ± 1.50 b167.51 ± 1.44 a†168.22 ± 0.91 a163.84 ± 0.99 c†
Tg (°C) *41.645 ± 2.28 a†50.26 ± 1.54 a†42.22 ± 4.50 a†47.70 ± 1.04 a†46.78 ± 0.55 c†46.53 ± 0.85 c†49.99 ± 0.90 b†52.96 ± 1.37 a†
* a–d Means carrying similar letters in a row of a particular time are statistically non-significantly different from each other. Means with the same symbol within a row indicate statistically significant differences at the same UAEOP ratios (p < 0.05).
Table 3. Thermogravimetric analysis (TGA) results of okra polysaccharides obtained under different UAE conditions.
Table 3. Thermogravimetric analysis (TGA) results of okra polysaccharides obtained under different UAE conditions.
Solid/Solvent RatioDegradation StageTpeak (°C)Weight Loss (%)Residue (%)
1:10 g/mLI84.8614.2327.48
II279.5758.29
1:25 g/mLI84.8612.7816.74
II281.5870.48
1:30 g/mLI83.8512.916.81
II280.5770.29
1:50 g/mLI89.913.3526.06
II280.5760.59
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Öncü Glaue, Ş.; Akcan, T.; Tavman, Ş. Thermal Properties of Ultrasound-Extracted Okra Mucilage. Appl. Sci. 2023, 13, 6762. https://doi.org/10.3390/app13116762

AMA Style

Öncü Glaue Ş, Akcan T, Tavman Ş. Thermal Properties of Ultrasound-Extracted Okra Mucilage. Applied Sciences. 2023; 13(11):6762. https://doi.org/10.3390/app13116762

Chicago/Turabian Style

Öncü Glaue, Şelale, Tolga Akcan, and Şebnem Tavman. 2023. "Thermal Properties of Ultrasound-Extracted Okra Mucilage" Applied Sciences 13, no. 11: 6762. https://doi.org/10.3390/app13116762

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