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Preparation of Turmeric Powder With Various Extraction and Drying Methods
Preparation of Turmeric Powder With Various Extraction and Drying Methods
(2022) 9:39
https://doi.org/10.1186/s40538-022-00307-1
Abstract
Background: In this study, turmeric (Curcuma longa L.) powder was prepared with various extraction and drying
methods. Extractions were performed using three solvents (water, 50% ethanol, and 70% ethanol) and three drying
methods, namely, spray drying (SD), freeze drying (FD), and spray-freeze drying (SFD).
Results: Levels of the curcuminoids, curcumin, demethoxycurcumin, and bisdemethoxycurcumin, in turmeric
powder preparations were analysed using HPLC, and scanning electron microscopy and laser particle size analysis
were used to observe and estimate the surface and size distribution of particles. The total amount of curcuminoids
ranged from 0.59–14.35 mg/g turmeric powder, and as the concentration of ethanol increased, the level of curcumi‑
noids, antioxidant activity, and average particle size significantly increased (all p < 0.05). In addition, the abundance
of curcuminoids significantly increased in the order of SFD, FD, and SD (p < 0.05), whereas the average particle size
significantly increased in the order of FD, SFD, and SD (p < 0.05).
Conclusions: The highest TPC and TFC were detected in SFD turmeric powder preparations, whereas the average
particle size significantly increased in the order of FD, SFD, and SD. Based on this study, we also showed that the level
of curcuminoids, antioxidant activity, TPC, TFC, and average particle size were most affected by the extraction solvent.
Keywords: Curcuma longa L., Curcuminoids, Extraction, Drying method, Antioxidant activity, Particle
*Correspondence: kwglee@dongguk.edu
1
Department of Food Science and Biotechnology, Dongguk University-Seoul,
32, Dongguk‑ro, Ilsandong‑gu, Goyang‑si, Gyeonggi‑do 10326, Republic
of Korea
Full list of author information is available at the end of the article
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Park et al. Chem. Biol. Technol. Agric. (2022) 9:39 Page 2 of 9
Graphical Abstract
Materials and methods for 3 h at 50 °C. After the addition of PSA (0.2 g), the
Chemical reagents and materials extract was then centrifuged at 14,000 × g and 4 °C for
Commercial grinded turmeric (Curcuma longa L.) was 15 min. The supernatant was filtered through a 0.45 µm
provided by Jindo Nonghyup in Korea. HPLC-grade nylon filter.
water, methanol, acetic acid, chloroform, and acetoni- Curcuminoid qualification was performed using thin
trile were purchased from J. T. Baker (Philipsburg, layer chromatography (TLC) and HPLC. For TLC, 20
NJ, USA). CUR (98% purity), DMC (95% purity), and μL of sample was manually spotted on a pre-coated sil-
BDMC (95% purity) were purchased from Supelco ica gel 60-F254 aluminium plate. The distance between
Corp. (Bellefonte, PA, USA). Primary secondary amine each spot was 1 cm. The plate was dried at room tem-
(PSA) was purchased from Agilent (Santa Clara, CA, perature and then developed in a TLC chamber previ-
USA), whereas Folin–Ciocalteu reagent and the anti- ously saturated with chloroform: methanol (47:3, v/v).
oxidant activity reagents 2,2-diphenyl-1-picrylhydrazyl Bands were scanned at 365 nm. The conditions of HPLC
(DPPH) and 2,2’-azino-bis (3-ethylbenzothiazoline- was optimized based on [14]. HPLC was performed using
6-sulfonic acid) (ABTS) were purchased from Sigma- a 1200 Series Gradient system (Agilent Technologies,
Aldrich Chemical Co. (St. Louis, MO, USA). All Santa Clara, CA, USA) equipped with a UV–VIS detector
chemicals and reagents used in the study were analyti- (UVD). The separation of curcuminoids was performed
cal grade. using octadecyl-silica (C18) (4.6 × 250 mm, 5 μm). The
column temperature was set at 30 °C, and 2% acetic acid
The extraction process (45% acetonitrile) was used as the mobile phase. The flow
The extraction process was modified from the previous rate was constant at 1 mL/min, and the injection volume
study [13]. Ground turmeric (50 g) was extracted with was 20 μL. The detection wavelength was 425 nm.
500 mL of water, 50% ethanol, or 70% ethanol for 2 h at
100 °C. The extract was centrifuged at 6500 ×g and 4 °C Analysis of antioxidant activity
for 10 min, and the supernatant was filtered through fil- The antioxidant activity of turmeric powder preparations
ter paper (No. 3, 110 mm, Whatman). The filtered solu- was determined using DPPH and ABTS assays.
tion was concentrated using a rotary evaporator under
reduced pressure at 60 °C to remove ethanol. DPPH assay
The DPPH free radical scavenging activity of extracted
The drying process samples was determined according to [15]. DPPH rea-
SD, FD, and SFD process were followed by the previ- gent (0.1 mmol L −1) was diluted with methanol to obtain
ous reports [9–12]. SD was performed in a B-290 spray an absorbance of 1.0 ± 0.02 at 517 nm using a spectro-
dryer (Buchi, Flawil, Switzerland). The extract was fed photometer. The DPPH solution (2.9 mL) was mixed with
into the chamber using a peristaltic pump, control- 0.1 mL of turmeric powder dissolved in methanol and
ling the feed flow rate using the pump rotation speed. then incubated for 30 min in the dark. The absorbance
The air and feed flow rates were 5 bars and 10 mL/min, at 517 nm was determined using an UV-1800 spectro-
respectively. The inlet and outlet temperatures were photometer (Shimadzu, Kyoto, Japan). Ascorbic acid was
150 °C and 85 °C, respectively. used as a positive control. The percentage of DPPH inhi-
For FD, the extract was frozen in an SE-45 deep bition was calculated using the following equation:
freezer (Tefcold, Viborg, Denmark) at − 80 °C for more % DPPH radical scavenging activity = [(Absblank–
than 24 h and then dried using a FD 8508 freeze dryer Abssample)/Absblank] × 100where Absblank and Abssample
(Ilsin Lab Co., Seoul, Korea) at− 70 °C and under 5 are the absorbance values of methanol and sample,
mTorr pressure for 7 days. respectively.
For SFD, the solution was sprayed with a feed rate of
43 mL/min and immediately frozen in liquid nitrogen. ABTS assay
Drying was performed at a pressure of 0.05 mbar. The The ABTS cation radical scavenging assay was followed
shelf temperature was kept at− 20 °C for 28 h and was [16]. ABTS reagent (7.4 mmol L−1) and potassium per-
then increased to 20 °C for 16 h. Before analysis, dried sulfate solution (2.6 mmol L −1) were mixed in equal
powders were stored at− 80 °C in a deep freezer. amounts and reacted in the dark at room temperature
for 16 h. Next, ABTS solution (1 mL) was diluted with
Analysis of curcuminoids methanol to obtain an absorbance of 1.0 ± 0.02 at 734 nm
Sample and ethanol were added to a 50 mL teflon cen- using a spectrophotometer. ABTS solution (2850 µL)
trifuge tube, and ultrasonic extraction was performed was mixed with 150 µL of turmeric powder dissolved in
methanol and then incubated for 2 h in the dark. The
Park et al. Chem. Biol. Technol. Agric. (2022) 9:39 Page 4 of 9
absorbance was measurement at 734 nm, and ascorbic particle size distribution. Turmeric powder (10 mg) was
acid was used as a positive control. The percentage of interspersed in 40 mL of water and then analysed.
ABTS inhibition was calculated as follows:
% ABTS radical scavenging activity = [(Absblank– Statistical analysis
Abssample)/Absblank] × 100where Absblank and
Abssample All analyses in this study were performed in triplicate and
are the absorbance values of methanol and sample, expressed as mean ± standard deviation (SD). Compari-
respectively. sons were performed by analysis of variance (ANOVA),
followed by Duncan’s multiple range test using IBM SPSS
Analysis of total polyphenol content (TPC) and total Statistics for Windows version 25 (IBM Corp., Armonk,
flavonoid content (TFC) NY, USA). Principal component analysis (PCA) was per-
Sample extraction for analysis of TPC and TFC formed to visualise the distribution of samples accord-
The method of extraction was similar to the method of ing to the various extraction and drying methods using
[17]. Turmeric powder was extracted with 10 mL of XLSTAT (Addinsoft, New York, NY, USA). A p value less
methanol: water (80:20) and stirred for 12 h. The extract than 0.05 was considered statistically significant.
was then re-extracted with 10 mL of the same solvent
and filtered through a 0.45 μm nylon filter. Results and discussion
Analysis of curcuminoids by TLC and HPLC
TPC Additional file 1: Fig. S1 shows the TLC analysis of each
Folin–Ciocalteu reagent was used for TPC according to sample’s result using an UV lamp. The chromatogram of
[18]. The extract (300 μL) was mixed with 2250 μL of 10% curcuminoids using HPLC–UVD is shown in Additional
Folin–Ciocalteu reagent. After 5 min of equilibrium, 6% file 1: Fig. S2. The calibration curve of each curcuminoid
sodium carbonate solution (2250 μL) was added. After (CUR, DMC, and BDMC) showed good linearity (all
90 min of reaction, absorbance was measured at 725 nm R2 = 1.000) at a concentration range of 0.1 − 25.00 µg/
using a spectrophotometer. A calibration curve of gallic mL. The content of curcuminoids in our turmeric pow-
acid was prepared, and the result was expressed as milli- der preparations is shown in Table 1. The total amount
gram of gallic acid equivalent per gram of turmeric pow- of curcuminoids ranged from 0.945–14.21 mg/g turmeric
der (mg GAE/g turmeric powder). powder, and the level of CUR, DMC, and BDMC ranged
from 0.611–9.443, 0.182–2.704, and 0.151–2.06 mg/g
TFC turmeric powder, respectively. We found that the cur-
The total flavonoid content was determined using the cuminoid with the highest content was CUR, whereas
colourimetric method described by [19]. For TFC, the the lowest content was BDMC. These findings are similar
extract (1000 μL) was mixed with 400 μL of 5% sodium to those reported in a previous study [6]. Furthermore,
nitrate. The mixture was allowed to stand for 6 min, the abundance of CUR was approximately 4 to 10 times
followed by the addition of 10% aluminium chloride higher than DMC and BDMC in turmeric powder.
(400 μL). After 6 min, 4% sodium hydroxide (4000 μL) Curcuminoid extraction is greater in ethanol than
was added. Methanol was used to adjust the volume to in water. In this study, the content of curcuminoids
10 mL. Next, the mixture was incubated for 15 min and increased significantly with higher ethanol concentra-
absorbance was measured at 510 nm using a spectropho- tion in the extraction solvent for each drying method (all
tometer. A calibration curve of quercetin was prepared, p < 0.05). Furthermore, the abundance of curcuminoids
and the result was expressed as milligram of quercetin significantly increased in the order of SFD, FD, and SD
equivalent per gram of turmeric powder (mg QCE/g tur- (p < 0.05). In the various previous reports, curcuminoids
meric powder). are efficiently extracted in organic solvents [20], whereas
heat treatment of turmeric results in a significant loss
Scanning electron microscopy (SEM) [21, 22].
The particle surface was observed by SEM using an
EM-30 scanning electron microscope from COXEM Analysis of antioxidant activity, TPC, and TFC
(Daejeon, Korea). Each dried powder was mounted on an Turmeric is rich in phenolic compounds, and the anti-
aluminium stage using carbon tape and then coated with oxidant activity of turmeric has been intensively stud-
gold for 3 min. ied [23–25]. Both polyphenol compounds and flavonoid
compounds have a major influence on determining anti-
Analysis of particle size distribution oxidant activity [26].
A laser particle size analyser (Mastersizer 3000, Mal- The antioxidant activities of nine turmeric powder
vern Panalytical, Malvern, UK) was used to measure the preparations were measured by DPPH and ABTS assays
Park et al. Chem. Biol. Technol. Agric. (2022) 9:39 Page 5 of 9
Table 1 Concentration of curcuminoids in turmeric powder according to the various extract and drying methods
Sample type Curcuminoids (mg/g turmeric powder)
CUR DMC BDMC Total
Table 2 Antioxidant activities in turmeric powder according to Table 3 Contents of total phenolics, total flavonoids content
the various extract and drying methods in turmeric powder according to the various extract and drying
methods
Sample type DPPH radical ABTS radical
scavenging activity scavenging Sample type TPC (mg GAE/g TFC (mg QCE/g
activity turmeric powder) turmeric powder)
Control 8 ± 1a 14.8 ± 0.8a Control 8.7 ± 0.3a 9.5 ± 0.8a
Spray drying Spray drying
Water 8.5 ± 0.9a 27.9 ± 0.8b Water 10.8 ± 0.4b 10.9 ± 0.6a
b c
50% ethanol 17.7 ± 0.9 62 ± 2 50% ethanol 30 ± 1 d
43 ± 1b
Freeze drying Freeze drying
Water 8 ± 1a 29.6 ± 0.7b Water 13.4 ± 0.4c 9.4 ± 0.7a
b c
50% ethanol 17 ± 1 62 ± 3 50% ethanol 32 ± 2e
43 ± 2b
c d
70% ethanol 23 ± 1 67 ± 3 70% ethanol 36.9 ± 0.2 f
69 ± 1d
Spray-freeze drying Spray-freeze drying
Water 9 ± 1a 26.0 ± 0.9b Water 13 ± 1c 10.4 ± 0.8a
b c
50% ethanol 16 ± 1 59 ± 2 50% ethanol 32 ± 1 e
47 ± 2c
c d
70% ethanol 25 ± 2 68 ± 4 70% ethanol 38.6 ± 0.2g 71.8 ± 0.7e
Ascorbic acid 40 ± 2d 98 ± 4e
1) All values are represented as mean ± standard deviation (S.D.) (n = 3)
1) All values are represented as mean ± standard deviation (S.D.) (n = 3) 2) Different superscript letters in the same column denote significant differences
2) Different superscript letters in the same column denote significant differences (Duncan’s range test, p < 0.05)
(Duncan’s range test, p < 0.05)
sample extracted using 70% ethanol. Water is not an effi- Table 4 Particle sizes (diameter, μm) in turmeric powder
cient solvent, because polyphenol compounds are more according to the various extract and drying method
soluble in less polar solvents than water [29]. Although Sample type Mean (μm) Median (μm)
curcuminoids are not classified as flavonoids, they react
similarly as flavonoid compounds to the aluminium chlo- Control 102.72 51.36
ride (AlCl3) used in the TFC method [30]. The principle Spray drying
in determining TFC is that AlCl3 forms acid-stable com- Water 1.21 0.61
plexes with the keto and hydroxyl groups of flavonoids 50% ethanol 23.36 11.68
(Additional file 1: Fig. S3). Curcuminoids are natural dia- Freeze drying
rylheptanoids, which consist of two aromatic o-methoxy Water 13.81 6.91
phenolic groups linked by a seven-carbon chain [30]. 50% ethanol 36.53 18.27
They exist in either the enol or keto form; however, the 70% ethanol 85.24 42.62
enol configuration is the major component in solution Spray-freeze drying
[31]. AlCl3 binds to curcuminoids through the β-diketone Water 5.86 2.93
group (Additional file 1: Fig. S4) [32]. 50% ethanol 28.30 14.15
70% ethanol 64.85 32.42
a b c
Fig. 1 Particle size distribution according to various extraction solvent and drying method. a Spray dried sample; (b) freeze dried sample; (c) spray
freeze dried sample; control; water extract; 50% ethanol extract; 70% ethanol extract
Park et al. Chem. Biol. Technol. Agric. (2022) 9:39 Page 7 of 9
Fig. 2 Scanning electron microscopy (SEM) image of various extraction solvents and drying methods. a Control; (b) WSD: water extract spray
drying; (c) 50ESD: 50% ethanol extract spray drying; (d) WFD: water extract freeze drying; (e) 50EFD: 50% ethanol extract freeze drying; (f) 70EFD:
70% ethanol extract freeze drying; (g) WSFD: water extract spray freeze drying; (h) 50ESFD: 50% ethanol extract spray freeze drying; (i) 70ESFD: 70%
ethanol extract spray freeze drying
TPC, and TFC, we found that turmeric powder extracted Additional file 1: Figure S1 TLC of turmeric powder according to the
various extract and drying methods. STD: Standard; WSD: Water extract
from 70% ethanol was the closest. Spray Drying; 50ESD: 50% Ethanol extract Spray Drying; WFD: Water
extract Freeze Drying; 50EFD: 50% Ethanol extract Freeze Drying; 70EFD:
70% Ethanol extract Freeze Drying; WSFD: Water extract Spray Freeze
Conclusions Drying; 50ESFD: 50% Ethanol extract Spray Freeze Drying; 70ESFD: 70%
In this study, we investigated the characteristics of tur- Ethanol extract Spray Freeze Drying. Figure S2 HPLC–UV chromatogram
meric powder prepared with three solvents (water, 50% of curcuminoids (Curcumin, Demethoxycurcumin, Bisdemethoxycur‑
cumin). Figure S3 Formation of flavonoid complex with AlCl3. Figure S4
ethanol, and 70% ethanol) and drying methods (SD, FD, Formation of curcumin complex with A lCl3. Figure S5 PCA of curcumi‑
and SFD). We determined the level of curcuminoids, noids, antioxidant activity, TPC, TFC, and particle size. WSD: water extract
antioxidant activity, TPC, TFC, and particle size in nine spray drying; 50ESD: 50% ethanol extract spray drying; WFD: water extract
freeze drying; 50EFD: 50% ethanol extract freeze drying; 70EFD: 70%
different samples, including control, and discovered, as ethanol extract freeze drying; WSFD: water extract spray-freeze drying;
the concentration of ethanol increased, the level of cur- 50ESFD: 50% ethanol extract spray-freeze drying; 70ESFD: 70% ethanol
cuminoids, antioxidant activity, TPC, TFC, and aver- extract spray-freeze drying.
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