Abstract
As a widely used spice, turmeric is rich in curcuminoids, which are known for their anti-inflammatory and antioxidant properties. However, the drying process, especially at high temperatures, often leads to significant curcumin degradation, impacting its bioactivity and quality. This study investigates drying turmeric using an innovative approach based on supercritical carbon dioxide (SC-CO2), and conventional drying methods (oven drying and freeze-drying) in terms of curcuminoid retention, color, solubility, chemical interactions, crystallinity, and morphology. The results revealed that SC-CO2 drying preserved up to 82.3 µg curcuminoids /mg dried turmeric, which was significantly higher than the levels retained by oven drying (55.4 µg/mg) and freeze-drying (42.4 µg/mg). Moreover, SC-CO2 drying exhibited better color retention, with higher L*, a*, and b* values compared to oven-dried samples. Further, SC-CO2 drying improved curcuminoids’ solubility (0.57 µg curcuminoids/mg turmeric) as compared to oven drying (0.29 µg/mg) and freeze-drying (0.12 µg/mg) at 60 °C, which is critical for enhancing curcumin bioavailability in food and pharmaceutical products. The morphological analysis showed that SC-CO2 drying maintained the structural integrity of turmeric better than the other methods, making it a promising technique for preventing thermal degradation and oxidation of micronutrients during drying.
Supplementary Information
The online version contains supplementary material available at 10.1038/s41598-025-18958-z.
Keywords: Turmeric, Curcumin, Curcuminoids, Supercritical carbon dioxide, Drying
Subject terms: Chemical engineering, Chemistry, Materials science
Introduction
Turmeric (Curcuma longa L.), a vibrant golden spice native to Southeast Asia and a member of the ginger family (Zingiberaceae), boasts a rich history dating back to Vedic times1,2. Renowned for its unique color, aroma, and flavor, turmeric has transcended its culinary role to become a revered medicinal spice. Its bioactive components, particularly curcuminoids, are credited with a number of health benefits, including potent anti-inflammatory and antioxidant properties1,3,4. However, to harness these therapeutic potentials and ensure long-term storage, fresh turmeric rhizomes necessitate proper drying.
Turmeric typically contains a high moisture content (~ 90%, wet basis), rendering it unsuitable for long-term storage without significant risk of spoilage5. Drying plays a crucial role in preserving the quality and bioactive compounds of turmeric. However, the drying method significantly impacts the final product’s physicochemical properties, particularly the retention of curcuminoids, the key bioactive components responsible for turmeric’s therapeutic effects1,6,7. Traditionally, sun drying has been the most widely used method for drying turmeric due to its simplicity and low cost. However, it offers minimal control over drying conditions (temperature, humidity, air circulation), exposing the product to potential contamination and uncontrolled light exposure. This often leads to significant curcumin degradation and inconsistent product quality. Alternative drying methods involve heated air, and can offer faster drying times. For example, Vallespir, et al.8 reported efficient low-temperature ultrasound-assisted convective drying of beetroot when combined with a freezing pre-treatment. Similarly, pulsed-spouted bed microwave freeze-drying reduced drying times and better preserved color and volatile compounds compared to conventional freeze-drying9. Despite these advances, microbiological safety remains a significant challenge for the drying industry10. Also, these methods result in non-homogeneity, overheating, discoloration, and deterioration, negatively impacting the quality of the dried materials1,11.
Supercritical carbon dioxide (SC-CO2) drying emerges as a promising alternative due to its unique properties. In this method, CO2 is pressurized (around 7.4 MPa) and heated (around 31 °C) to a supercritical state, where it acts like both a gas (for deep penetration) and a liquid (for efficient moisture removal). It retains the gas-like characteristic of high diffusivity, allowing for deep penetration into the cellular structure of food particles. Simultaneously, SC-CO2 possesses a liquid-like density, increasing its solvating power. This enables the removal of moisture in food items12,13. Furthermore, the low processing temperature minimizes thermal degradation, a major threat to heat-sensitive curcuminoids and the rapid drying times facilitated by SC-CO2 can significantly reduce/eliminate exposure to detrimental factors like light and oxygen14. Beyond its effectiveness, CO2 is a naturally occurring and non-toxic gas, and the closed-loop nature of the system allows for CO2 recycling and reuse, minimizing environmental impact.
Although SC-CO2 drying is well-established in the preparation of aerogels12, its use in food processing is still emerging, like carrots15, basil16, coriander17, apples14 and tropical fruits such as mangoes and persimmons18. These studies suggest that SC-CO2 drying can preserve the structural integrity and bioactive compounds effectively, but the processing parameters impact drying behavior. For example, Brown, et al.15 identified temperature as a critical factor influencing drying time, yet the interplay between temperature, pressure, and CO2 density on moisture diffusivity and matrix integrity requires further quantification. Also, Bušić, et al.16 demonstrated that both pressure and drying duration significantly influence the retention of bioactive compounds and sensory characteristics in dried basil, highlighting the sensitivity of phytochemicals to subtle process variations. Nevertheless, there is no report on drying turmeric using SC-CO2.
Therefore, the overall goal of this study was to investigate the impact of SC-CO2 drying on the properties of turmeric. The specific objectives included investigating the influence of different drying methods (SC-CO2, oven drying, and freeze-drying) on curcuminoids content, morphology, color, solubility, crystallinity, and chemical interactions.
Results and discussion
Turmeric samples were dried using oven, freeze, and SC-CO2 drying, where oven and freeze drying were employed as the conventional drying approaches1. While oven drying operates via temperature-induced vapor pressure gradients, it often results in significant degradation of thermolabile compounds, particularly curcuminoids in turmeric5. Freeze drying, proceeding through freezing (−40 °C to −50 °C) and sublimation under high vacuum (≤ 100 Pa), better preserves bioactive constituents but can compromise cellular integrity through ice crystal formation and growth19. SC-CO2 drying was conducted at 20 MPa And 60 °C based on our preliminary experiment and previous publications, for its superior mass transfer properties12. At this condition, SC-CO2 exhibits enhanced diffusivity and low surface tension, which enables efficient moisture removal15. Additionally, it prevents oxidative deterioration of bioactive compounds since no oxygen is involved during drying.
Moisture content
Table 1 presents the moisture content data of turmeric dried using oven, freeze, and SC-CO2 drying methods. The statistical analysis showed significant differences among the three drying techniques (p < 0.05). On average, oven-dried turmeric showed the highest moisture content (10.10 ± 0.04%), followed by SC-CO2 (9.45 ± 0.17%), and freeze-drying showed the lowest moisture content (8.97 ± 0.33%) (p < 0.05). The oven-drying and freeze-drying results were consistent with findings from other studies1,20,21. For instance, Malik and Kumar6 and Prasad, et al.20 reported similar moisture content ranges for oven-dried and solar-biomass dried turmeric (9–11%). A slightly lower moisture content (~ 5%) in solar conduction-dried samples was observed by Borah, et al.22. Furthermore, Llano, et al.1 revealed ~ 8% moisture content in turmeric dried using a traditional solar, convection oven, and fluidized bed drying. Overall, all three drying techniques were effective in reducing moisture content (< 10%) to levels suitable for preservation, typically below 9–10% for turmeric powder21.
Table 1.
The moisture content and water activity of turmeric dried by oven, freeze, and SC-CO2 drying methods.
| Drying method | Moisture content (%, wet basis) |
Water activity (aw) |
|---|---|---|
| Oven | 10.10 ± 0.04a | 0.54 ± 0.00c |
| Freeze | 8.97 ± 0.33b | 0.57 ± 0.01a |
| SC-CO2 | 9.45 ± 0.17ab | 0.55 ± 0.00b |
*Means in the same column that do not share a common letter are significantly different (p<0.05).
Additionally, the water activity (aw) values for all dried samples were below 0.6, which is the critical threshold for inhibiting microbial growth and ensuring product safety and shelf stability. Oven-dried turmeric exhibited the lowest aw (0.54 ± 0.00), followed closely by SC-CO2-dried (0.55 ± 0.00) and freeze-dried turmeric (0.57 ± 0.01). These results confirm that all drying methods effectively reduced water activity to safe levels, contributing to the microbial stability and prolonged shelf life of the turmeric powders23.
Color analysis
Table 2 shows significant variations in L* (lightness), a* (redness), and b* (yellowness) values of blanched fresh turmeric and dried turmeric using different methods (oven, freeze, and SC-CO2). The fresh (blanched) turmeric indicated a moderately light appearance (L* = 58.05 ± 0.22), redness (a* = 20.14 ± 0.18) and strong yellowness (b* = 47.92 ± 2.15), which are characteristic of turmeric’s vibrant golden-orange hue (Fig. 1)24. Freeze-dried turmeric exhibited the highest L* value (76.55 ± 0.04), indicating the lightest color, followed by SC-CO2 (72.71 ± 0.58) and oven-dried (63.83 ± 0.30) samples. SC-CO2 dried turmeric showed the highest a* value (20.35 ± 0.95), suggesting more redness, while freeze-dried samples had the lowest (11.86 ± 0.01) (p < 0.05). Similarly, Ray, et al.25 reported a redness value of around 10–15 in the solar, and hot air oven-dried turmeric. The b* values, representing yellowness, were the highest in freeze-dried samples (56.53 ± 0.07), followed by SC-CO2 (53.72 ± 0.15) and oven-dried (42.64 ± 0.28). Comparing the color changes (ΔE*), freeze drying caused the largest color difference from the fresh sample (ΔE* = 22.02), followed by SC-CO2 drying (ΔE* = 15.78), while oven drying resulted in the smallest color deviation (ΔE* = 8.23) from the original blanched color24,25. Ray, et al.25 revealed that high-temperature drying methods like oven drying (60 ℃) resulted in significant color degradation, causing intense Maillard reactions, oxidation, and structural changes in unblanched turmeric samples. In that study, the degradation was primarily attributed to the activity of polyphenol oxidase (PPO) and peroxidase (POD), leading to intense browning. However, in our study, since turmeric was blanched prior to drying, which reduced the enzymatic activity. According to Ray, et al.25 and Aksoy, et al.26 the superior color retention in freeze-dried samples was due to low-temperature drying methods, which probably better preserved heat-sensitive pigments like curcumin in turmeric; however, in our study, the porous structure of freeze-dried turmeric contributed to a higher lightness value, which in turn resulted in an increased ΔE* value. The intermediate color values of SC-CO2-dried turmeric suggest a trade-off between color preservation and processing efficiency, as noted by Pravallika, et al.27 on SC-CO2 drying of red bell pepper, apple pieces, and carrot slices.
Table 2.
The color parameters of turmeric dried by oven, freeze, and SC-CO2 drying methods.
| Samples | L* | a* | b* | ΔE* | C | H⁰ |
|---|---|---|---|---|---|---|
| Fresh | 58.05 ± 0.22d | 20.14 ± 0.18a | 47.92 ± 2.15c | N/A | 51.99 ± 1.91b | 22.83 ± 1.11a |
| Oven-dried | 63.83 ± 0.30c | 17.64 ± 0.14b | 42.64 ± 0.28d | 8.23 ± 0.27c | 46.14 ± 0.29c | 22.48 ± 0.14a |
| Freeze-dried | 76.55 ± 0.04a | 11.86 ± 0.01c | 56.53 ± 0.07a | 22.02 ± 0.07a | 57.76 ± 0.07a | 11.85 ± 0.03b |
| SC-CO2-dried | 72.71 ± 0.58b | 20.35 ± 0.95a | 53.72 ± 0.15b | 15.78 ± 0.57b | 57.45 ± 0.21a | 20.75 ± 0.94a |
*Means that do not share a common letter within the same column are significantly different (p<0.05). Fresh: The color of fresh samples after blanching (prior to drying) was reported.
Fig. 1.
Photographs of turmeric powders dried by (a) oven, (b) freeze, and (c) SC-CO2 drying methods.
Chroma (C) values, which indicate color saturation and vividness, decreased after oven drying (46.14), whereas freeze drying (57.76) and SC-CO2 drying (57.45) maintained or slightly enhanced the chroma compared to the fresh sample (51.99), indicating superior retention of color intensity by the latter two methods. Further, the hue angle (H°) of fresh turmeric was 22.83°, indicating a reddish-orange tone. After drying, H° decreased slightly to 22.48° (oven-dried), 20.75° (SC-CO2-dried), and 11.85° (freeze-dried). These shifts suggest a minor yet noticeable color change, especially in the freeze-dried sample, which may be due to altered pigment stability or microstructural differences. The reduction in H° across all drying methods signifies a deepening of color, potentially influenced by non-enzymatic browning or concentration of pigments during moisture loss28.
Curcuminoid content
Table 3 compares the total and individual curcuminoid levels (BDMC, DMC, and CUR) in fresh turmeric versus dried turmeric, with the latter being dried using different methods. The fresh turmeric yielded the highest total curcuminoid content (95.62 ± 6.17 µg/mg on a dry basis). A very close curcumin content of 94 µg/mg in fresh turmeric was reported by Hirun, et al.23. Furthermore, SC-CO2 drying closely followed (82.30 ± 1.88 µg/mg) with a nonsignificant difference from the fresh sample (p > 0.05). This demonstrates its efficacy in preserving curcuminoids, potentially attributable to the acidic environment of SC-CO2, where curcumin is more stable, and the lack of oxygen in the drying environment29. Additionally, in the SC-CO2 dried sample, BDMC was the only curcumin moiety (26.39 ± 0.59 µg/mg) showing a significantly lower amount compared to fresh turmeric (39.21 ± 2.75 µg/mg) (p < 0.05). Therefore, SC-CO2 drying demonstrated a superior capacity for preserving curcuminoids with methoxy groups (DMC and CUR) compared to other drying methods. Although BDMC lacks potentially reactive methoxy groups, it may still undergo degradation processes, with pressure and temperature having a significant impact on its recovery30. Furthermore, no significant differences were detected in the levels of the curcuminoids between oven and freeze-drying (p > 0.05). Oven drying (55.35 ± 8.10 µg/mg) likely caused significant thermal degradation, while freeze-drying (42.35 ± 8.70 µg/mg) may have led to structural changes affecting extractability. This aligns with findings by Suresh, et al.31 and Bambirra, et al.32who reported thermal degradation of curcumin during cooking. A previous study indicated that in the process of SC-CO2 drying, CO2 penetrates the food and avoids the formation of the vapor-liquid interfaces14. Initially, it eliminates free water, which is easily extractable, then proceeds to penetrate deeper into the food to remove entrapped water.
Table 3.
The curcuminoid levels in fresh turmeric and oven-, freeze-, and SC-CO2-dried turmeric samples.
| Turmeric samples | Total Curcuminoids (µg/mg sample) | BDMC (µg/mg sample) |
DMC (µg/mg sample) |
CUR (µg/mg sample) |
|---|---|---|---|---|
| Fresh | 95.62 ± 6.17a | 39.21 ± 2.75a | 20.35 ± 1.18a | 36.03 ± 2.43a |
| Oven-dried | 55.35 ± 8.10b | 15.39 ± 1.99c | 11.75 ± 1.65b | 28.21 ± 4.46ab |
| Freeze-dried | 42.35 ± 8.70b | 14.16 ± 2.80c | 8.98 ± 1.83b | 19.21 ± 4.07b |
| SC-CO2-dried | 82.30 ± 1.88a | 26.39 ± 0.59b | 20.37 ± 0.95a | 35.53 ± 0.35a |
BDMC: Bisdemethoxycurcumin, DMC: Demethoxycurcumin, CUR: Curcumin.
*Means that do not share a common letter within the same column are significantly different (p<0.05).
Water solubility of curcuminoids
Figure 2 and Fig. S1 show the water solubility and chromatograms, respectively, of curcuminoids in turmeric dried using oven, freeze, and SC-CO2 drying. SC-CO2 drying revealed superior curcuminoids’ solubility (0.25 ± 0.01 µg curcuminoids/mg turmeric at 23 °C, And 0.57 ± 0.01 µg curcuminoids/mg turmeric at 60 °C), followed by oven drying (0.07 ± 0.01 µg curcuminoids/mg turmeric at 23 °C, And 0.29 ± 0.01 µg curcuminoids/mg turmeric at 60 °C), while freeze-drying showed the lowest solubility (0.02 ± 0.01 µg curcuminoids/mg turmeric at 23 °C, And 0.12 ± 0.02 µg curcuminoids/mg turmeric at 60 °C) (p < 0.05). The highest water solubility of curcuminoids in SC-CO2-dried turmeric might be due to higher curcuminoid retention, an open porous structure that increases water interaction, intermolecular interactions, and reduced crystallinity. In contrast, freeze-dried turmeric exhibited the lowest solubility because of its lower curcuminoids retention. The lower solubility of oven-dried could be attributed to thermal degradation, oxidation, or structural changes in curcumin, as suggested by Guo, et al.33 and Emelike34.
Fig. 2.
Water solubility (µg curcuminoids/mg sample) of turmeric dried by (a) oven, (b) freeze, and (c) SC-CO2 drying methods.
All drying methods exhibited significantly enhanced solubilities at elevated temperature (60 °C) compared to room temperature (23 °C) (p < 0.05), with SC-CO2 drying demonstrating a 2.24-fold increase, oven drying a 4.14-fold increase, and freeze-drying a 6-fold increase at 60 °C. As expected, at higher temperatures, the thermal energy disrupts intramolecular hydrogen bonds and intermolecular forces, exposing polar hydroxyl (− OH) and keto (> C═O) groups, which increase the availability and solubility of curcumin in water29. The higher temperature (60 vs. 23 °C) might alter the intermolecular forces between curcuminoids and other compounds in turmeric, potentially improving its solubility35. These results highlight the complex interaction between drying methods and temperature on the water solubility of curcuminoids in turmeric and emphasize the need to consider both factors in applications where solubility is important, such as food processing or pharmaceutical formulations.
Morphology
Figure 3 presents morphological changes in turmeric dried using oven drying, freeze drying, and SC-CO2 drying. In the oven-dried turmeric (Fig. 3A, a), strong capillary forces and high surface tension during water removal resulted in a more compact and fused structure with less porosity as the liquid-vapor interface induced significant compressive stresses on cell walls. This aligns with findings by Karam, et al.36 who observed that thermal drying could lead to shrinkage and collapse of cellular structures. The freeze-dried turmeric (Fig. 3B, b) exhibited a more open, porous structure with sheet-like formations, where ice crystal formation and sublimation created a highly macroporous structure by bypassing liquid-phase surface tension effects27,36,37. Furthermore, the SC-CO2 dried sample (Fig. 3C, c) showed a preserved microstructure due to near-zero surface tension in the supercritical state, which eliminated capillary stresses during water removal. Similarly, Pravallika, et al.27, Ubeyitogullari and Ciftci38, and Ahmadzadeh and Ubeyitogullari39 found that SC-CO2 drying can preserve structural integrity better than air drying or freeze-drying. The differences in microstructure could significantly impact properties such as flowability, rehydration capacity, and bioactive compound bioaccessibility. For instance, the more open structure may contribute to better solubility, as noted by Karam, et al.36 and Kaur, et al.12 while the compact structure might result in slower dissolution27,36. This open porous structure contributed to the increased water solubility of SC-CO2-dried turmeric, as reported in Fig. 2. In addition to morphological differences, the drying method can induce structural transformations in curcumin itself. Thermal drying may lead to partial degradation or isomerization of curcumin molecules, potentially reducing their antioxidant activity. Freeze drying, although less harsh, may still promote crystalline formation that can limit curcumin solubility36. SC-CO2 drying, on the other hand, may help retain curcumin in a more amorphous state with fewer crystalline domains due to its low-temperature and low-stress mechanism. This amorphization can enhance curcumin’s water dispersibility, and overall functional performance in food and nutraceutical applications27.
Fig. 3.
SEM images of turmeric dried by (A, a) oven, (B, b) freeze, and (C, c) SC-CO2 drying methods. Uppercase letters represent the images captured at a lower magnification, while lowercase letters represent the images captured at a higher magnification.
Crystallinity
XRD patterns of turmeric samples showed peaks at 2θ 15°, 17°, 22° And 25°40. Amalraj, et al.41 revealed the XRD peaks of curcuminoids exist between 2θ 5–30°. Oven-dried turmeric samples showed the highest intensity peaks (Fig. 4), indicating a more crystalline structure with 9.5% crystallinity, and freeze-dried sample revealed a crystallinity of 8.3%. The SC-CO2 dried samples showed a crystallinity of 7.5%, indicating a dominant amorphous structure12. The differences in crystallinity can significantly influence the key properties such as solubility, stability, and bioavailability42,43. For instance, the more amorphous structure of SC-CO2 dried turmeric might have contributed to its higher solubility, as observed in the solubility data (Fig. 2).
Fig. 4.
XRD patterns of turmeric powders dried by (a) oven, (b) freeze, and (c) SC-CO2 drying methods.
Chemical interactions
The FTIR spectra of turmeric subjected to different drying methods revealed broadly similar profiles (Fig. 5), indicating the major functional groups in curcuminoids and other polymers. The broad absorption band at 3400–3200 cm−1, attributed to phenolic O-H stretching vibrations, was more intense and broadened in the oven-dried sample25,41. This broadness may be linked to increased hydrogen bonding due to heat-induced conformational changes that promote intermolecular interactions. This phenomenon is consistent with literature noting broadened O-H bands in formulations with polar-nonpolar layer interfaces due to hydrogen bonding among curcuminoids and surrounding matrices25,41,44. In contrast, both SC-CO2 and freeze-dried samples exhibited sharper and slightly blue-shifted O-H bands, indicating less extensive hydrogen bonding and better preservation of native phenolic structures. The strong and well-defined peaks in the aromatic C = C stretching region (1600–1500 cm−1), notably near 1602 cm−1 and 1510 cm−1, were most intense in SC-CO2 dried turmeric, suggesting minimal oxidation or degradation of the conjugated aromatic systems under non-thermal conditions25,44. In comparison, the oven-dried sample showed broader and less intense peaks in this region, likely reflecting partial structural degradation due to thermal stress and hydrogen bonding of curcuminoids between the polar-nonpolar layer41. Additional differentiation was observed in the 1200–1000 cm−1 region, associated with methoxy (C-OCH3) and ether (C-O-C) stretching vibrations. Peaks around 1281 cm−1 and 1027 cm−1 were clearer and more defined in SC-CO2 dried turmeric, consistent with improved retention of methoxylated and ether-linked groups. Moreover, characteristic bands around 714 cm−1 and 857 cm−1, which correspond to aromatic ring bending and phenyl ring vibrations in curcuminoids respectively, were better preserved in the SC-CO2-dried sample19,25,44. The curcuminoid standard spectrum served as a critical benchmark, displaying sharp, well-resolved peaks across all functional regions. Among the dried samples, SC-CO2-dried turmeric most closely resembled this standard in both peak position and resolution, indicating superior structural fidelity. In contrast, the oven- and freeze-dried samples showed more pronounced deviations, particularly in the phenolic and aromatic regions, likely due to heat or sublimation-induced molecular perturbations.
Fig. 5.
ATR-FTIR spectra of curcuminoid standard and turmeric powders dried by oven, freeze, and SC-CO2 drying methods.
Conclusions
This study demonstrates the advantages of SC-CO2 drying over traditional drying methods, namely oven drying and freeze drying, in preserving the quality and bioactive compounds of turmeric. Among the three drying methods, SC-CO2 drying showed the highest retention of curcuminoids (82.30 ± 1.88 µg/mg), closely matching the curcuminoid levels of fresh turmeric (95.62 ± 6.17 µg/mg). In comparison, oven drying and freeze drying resulted in much lower curcuminoid retention, at 55.35 ± 8.10 µg/mg and 42.35 ± 8.70 µg/mg, respectively. Additionally, SC-CO2 dried samples exhibited a lightness (L*) value of 72.71 ± 0.58, intermediate between freeze-dried samples (76.55 ± 0.04) and oven-dried samples (63.83 ± 0.30). The redness (a*) and yellowness (b*) values were highest in SC-CO2 dried turmeric (20.35 ± 0.95 and 53.72 ± 0.15, respectively), indicating better color retention. Moreover, SC-CO2 dried turmeric showed the highest curcuminoids solubility (0.57 µg curcuminoids/mg turmeric) at 60 °C, which was significantly higher than both freeze-dried (0.12 µg curcuminoids/mg turmeric) and oven-dried (0.29 µg curcuminoids/mg turmeric) turmeric samples at the same temperature. This might be due to the higher curcumin retention, more porous structure, intermolecular interactions, and reduced crystallinity of SC-CO2 dried turmeric. Overall, SC-CO2 drying offers significant improvements in the quality of dried turmeric, including higher curcuminoids retention, better color preservation, enhanced solubility, and favorable structural characteristics. This novel drying method has great potential for the food, nutraceutical, and pharmaceutical industries, particularly in the production of high-quality turmeric powders.
Methods
Materials
Turmeric (Curcuma Aromatica) was purchased from the Fijian Spice Company (NJ, USA). The curcuminoid standard (> 98%) (a mixture of BDMC: Bisdemethoxycurcumin (%2.5 ± 0.2), DMC: Demethoxycurcumin (%18.5 ± 0.1), and CUR: Curcumin (%78.9 ± 0.2)) and ethanol were purchased from Fisher Scientific (PA, USA), and liquid carbon dioxide (> 99.99%) was supplied by Airgas, Inc. (AR, USA).
Sample Preparation
The turmeric rhizomes were sliced into small pieces (1-cm thick) and blanched to eliminate enzyme activity. The blanching was conducted according to Ahmadzadeh, et al.45. Briefly, the turmeric samples were steam-blanched in a steamer (Dixie, M-6 Steam Blancher-Cooler) at 90 °C for 3 min. After blanching, the samples were prepared for drying. Fresh turmeric samples were manually minced with a knife for curcuminoids content analysis, and dried samples were ground using a coffee grinder and sieved through a #35 mesh (< 500 μm) for further analysis46.
Turmeric drying
Oven drying
The blanched turmeric samples (10 g) (1-cm thick) were spread on a perforated aluminum tray. The drying was conducted at 50 °C to a constant weight1.
Freeze-drying
The blanched turmeric samples (10 g) were packed into Ziploc bags and frozen for at least 24 h. Then, freeze-drying was conducted at − 45 °C and 7.3 Pa for 48 h using a freeze-dryer (Labconco, MO, USA).
SC-CO2 drying
The blanched turmeric samples were dried according to Kaur, et al.12 using a lab-scale SC-CO2 technology (SFT-120, Supercritical Fluid Technologies Inc., DE, USA). First, the samples were loaded into a thimble and placed in a 100 mL high-pressure vessel with glass wool placed on both ends of the vessel. The vessel and micrometering valve temperatures were set to 60 °C. The micrometering valve was heated to prevent freezing due to the Joule-Thomson effect. After the set temperatures were attained, the system was pressurized to 20 MPa. The SC-CO2 drying continued for 6 h with a CO2 flow rate of 3 L/min. Drying conditions for SC-CO2 were determined through preliminary experiments (pressure: 10–20 MPa, temperature: 40–60 °C, and CO2 flow rate 1–3 L/min) and literature12. After the drying process was finished, the system was depressurized. Finally, turmeric samples were collected and stored at room temperature (23 °C) in airtight containers.
Moisture content
The moisture content was determined according to the AACC 2000 method12.
Color analysis
The color parameters (i.e., L*, a*, and b* values) were determined using a colorimeter (Minolta CR-300, Konica Minolta, NJ, USA). Prior to analysis, the colorimeter was calibrated via a white calibration plate. The total color change (
) chroma (C) and hue angle (H°) were measured according to Eqs. 1, 2, and 3, repectively28,47.
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1 |
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2 |
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3 |
Curcuminoids content
Curcuminoids extraction and quantification were carried out according to the method described by Ubeyitogullari and Ciftci48. First, curcuminoids were extracted from turmeric samples by repeated solvent extraction. Briefly, a turmeric sample (5 mg) was suspended in 10 mL of acetonitrile and vortexed vigorously for 5 min. The suspension was centrifuged at 10,000g for 15 min, and the supernatant was collected. The procedure was repeated 4 times, and all the supernatants were pooled in a separate vial. The supernatants were analyzed using high-performance liquid chromatography (Shimadzu Corp., Japan), equipped with an SPD-20AV UV/VIS detector, a SIL—10AF autosampler, and a CTO-20 A column oven. Briefly, a sample (20 µL) was introduced into a reversed-phase Gemini C18 110 A column (150 × 4.6 mm, 5 μm; Phenomenex, CA, USA) using a flow rate of 0.8 mL/min, and the temperature was held at 30 °C. The isocratic elution was conducted using mobile phases of acetonitrile (A) And 5% acetic acid (B) at a ratio of 45:55 (v/v). Elution was monitored at 420 nm, and curcumin was quantified using a calibration curve (R2 = 0.9999) generated with an authentic standard (ranging from 0.78 to 100 µg/mL in acetonitrile).
Curcuminoids solubility
The turmeric solubility was conducted at room temperature (23 °C) and at a potential processing temperature (60 °C)12. Briefly, the sample (1 g) was mixed with deionized water (12 mL) in a 50 mL falcon tube for 1 min using a vortex mixer. The mixture was then subjected to an orbital shaker (VMR DS-500E orbital shaker, Henry Troemner LLC, USA) for 30 min before centrifugation at 3,000 rpm for 10 min. For the processing temperature, the samples were kept in a water bath at 60 ℃ for 10 min prior to centrifugation. The resulting supernatant was collected and filtered to determine curcuminoids content using the HPLC method described above.
Morphology
A scanning electron microscope (SEM, FEI NovaNanoLab200 Dual-Beam system, FEI company, OR, USA) was used to determine the surface morphology of the dried turmeric samples49. Prior to imaging, the samples were coated with a gold layer using a sputter-coater (EMITECH SC7620 Sputter Coater, MA, USA). Then, imaging was conducted using the vacuum mode at 5 mm working distance, 15 kV, and 15 mA.
XRD
The XRD patterns were recorded using an X-ray diffractometer (PW3040X`PertMRD, Philips, Almelo, Netherlands). The powdered samples were scanned at 45 kV and 40 mA at a range of 5–40° with a step size of 0.02⁰/s. The area under the relevant curves was calculated using OriginLab 2021 (OriginLab Corporation, MA, USA). The percent degree of crystallinity was calculated using Eq. 2.
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FTIR
Fourier transform infrared spectroscopy (FTIR, IRAffinity-IS Fourier transform infrared spectrometer, SHIMADZU Corp., Kyoto, Japan) was used to survey the chemical interactions in the samples. The FTIR was equipped with a Quest attenuated total reflectance (ATR) accessory (Specac Company, Orpington, UK). The samples were scanned between 400 and 4000 cm−1 wavenumbers at a resolution of 4 cm with 64 scans.
Statistical analysis
The statistical Analysis was performed in JMP Pro 17.0 (SAS Institute, NC, USA) using ANOVA and Tukey’s HSD test with a 5% significance level. The results were expressed as the mean ± standard deviation with three replicates per sample.
Supplementary Information
Below is the link to the electronic supplementary material.
Acknowledgements
This work was supported by McCormick Science Institute. This project was also supported, at least in part, by the USDA National Institute of Food and Agriculture, Multistate Project NC-1023, Accession number 1025907, and AFRI award no: 2023-67022-40164. We greatly appreciate Dr. Chris Mazzanti for helping with the FTIR analysis.
Abbreviations
- SC-CO2
Supercritical carbon dioxide
- SEM
Scanning Electron Microscopy
- XRD
X-Ray Diffractometer
- FT-IR
Fourier Transform Infrared
- BDMC
Bisdemethoxycurcumin
- DMC
Demethoxycurcumin
- CUR
Curcumin
Author contributions
Sumanjot Kaur: formal analysis, methodology, investigation, visualization, writing-original draft; Arda Tuhanioglu: formal analysis, methodology, investigation, writing-original draft; Ali Ubeyitogullari: conceptualization, methodology, investigation, resources, project administration, supervision, funding acquisition, writing-review & editing.
Data availability
All data generated or analysed during this study are included in this published article.
Declarations
Competing interests
The authors declare no competing interests.
Footnotes
Publisher’s note
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Data Availability Statement
All data generated or analysed during this study are included in this published article.









