Received: 13 July 2023 Revised: 22 September 2023
DOI: 10.1111/jfpe.14479
ORIGINAL ARTICLE
A novel approach for sterilization and concentration of
traditional functional drinks: Membrane-based nonthermal
processes
Fahliza Meutia 1 | C. Hanny Wijaya 2
1
Faculty of Industrial Technology, Department
of Chemical Engineering, Bandung Institute of
Technology, Bandung, Indonesia
2
Faculty of Agricultural Technology,
Department of Food Science and Technology,
IPB University, Bogor, Indonesia
Correspondence
Helen Julian, Faculty of Industrial Technology,
Department of Chemical Engineering, Bandung
Institute of Technology, Bandung 40132,
Indonesia.
Email: helen_j@office.itb.ac.id
Funding information
Institut Teknologi Bandung
J Food Process Eng. 2023;46:e14479.
https://doi.org/10.1111/jfpe.14479
Accepted: 6 October 2023
| Helen Julian 1
Abstract
The applicability of microfiltration (MF) and osmotic membrane distillation (OMD)
for sterilization and concentration of traditional functional drink constituents, such
as Curcuma xanthorrhiza, ginger, lime, Java tea, and sappan wood extracts, was eval-
uated in this study. MF showed excellent performance in microorganisms elimina-
tion, turbidity reduction, and maintaining antihyperglycemic activity performance.
However, a reduction of total phenol and antioxidant activity were observed due to
the retention by MF. Fouling in MF was challenging and resulted in rapid flux
decline. The concentration of sterilized extracts by OMD operation resulted in a
concentration factor of 1.15, 1.13, 1.10, 1.24, and 1.24 for ginger, lime,
C. xanthorrhiza, Java tea, and sappan wood, respectively. The active compounds
were well preserved, with a maximum of 20% reduction compared to sterilized
extracts. Despite insignificant foulant deposition, the OMD flux in tests using
C. xanthorrhiza, ginger, and lime as the feed decreased over time, indicating reduced
driving force.
Practical applications
The application of membrane technology for juices and liquid foods sterilization and
concentration has been widely researched. In this research, we evaluated the perfor-
mance of MF and OMD for the sterilization and concentration of traditional func-
tional drinks. The results indicated that the functional drink can be sterilized by MF
with excellent preservation of the active compounds, such as those responsible for
the antihyperglycemic and antioxidant activities. The OMD could also concentrate
the traditional functional drink, even though concentration polarization posed a chal-
lenge to flux stability. The degradation of phenolic compounds and antioxidant activ-
ity of the concentrated traditional functional drink was at a minimal value, indicating
the promising application of MF and OMD. We believe this article provides new and
exciting insights to push forward the sterilization and concentration process in indus-
trial scale.
KEYWORDS
beverage concentration, functional drink, microfiltration, osmotic membrane distillation,
sterilization
wileyonlinelibrary.com/journal/jfpe © 2023 Wiley Periodicals LLC. 1 of 15

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1 | I N T RO DU CT I O N
Functional foods are foods whose contents are good for improving
physiological functions and reducing diseases, as demonstrated by
various studies that indicate benefits when consumed on a daily basis.
Functional drinks are beverages that are specifically formulated to
deliver a specific health or wellness benefit beyond basic hydration.
They typically contain added ingredients such as vitamins, minerals,
herbs, amino acids, and other nutrients that are intended to improve
physical or cognitive performance, boost energy, support digestion,
enhance immunity, or address specific health conditions (Alongi &
Anese, 2021; Nazir et al., 2019). In Southeast Asia, traditional func-
tional drinks have been used for centuries as an herbal medicine with
various unique blends of ingredients, typically made from mostly natu-
ral ingredients such as herbs, spices, and other plant-based products.
Several ingredients widely used in the developed traditional functional
drinks are Java tea, sappan wood, Curcuma xanthorrhiza, ginger, and
lime (Mardhiyyah et al., 2019; Wijaya et al., 2018). Java tea is a plant
native to Southeast Asia that is believed to have diuretic, anti-
inflammatory, and antibacterial properties. It is also a natural remedy
for conditions such as urinary tract infections and liver and gallbladder
problems (Indariani et al., 2014; Michael et al., 2018). The heartwood
of the sappan wood tree has been used for centuries to improve cir-
culation, reduce inflammation, and boost the immune system (Wijaya
et al., 2018). Sappan wood contains phytochemical compounds such
as tannin, resin, gallic acid, resorcin, brazilein, brazilin, quercetin, and
essential oil. Brazilin, in particular, acts as an antioxidant and can
effectively reduce blood glucose levels. Quercetin is the component
in sappan wood extract hypothesized to have movement antihyper-
glycemic (Indariani et al., 2014). Java tea and sappan wood are also
known for their antihyperglycemic activity, specifically beneficial for
diabetes prevention and maintaining sugar blood levels (Indariani
et al., 2014; Rekasih et al., 2021). C. xanthorrhiza is believed to have
anti-inflammatory, antioxidant, and antipyretic properties. Ginger has
a long history of use in traditional medicine for its purposed health
benefits, such as reducing nausea, pain, and inflammation and improv-
ing digestive function (Kusumawati et al., 2021). One of functional
drink based on Java tea based has been commercially produced with a
patented formulation (A'yuni et al., 2022; Wijaya et al., 2018, 2020).
This particular commercial functional drink consisted of Java tea, sap-
pan wood, C. xanthorrhiza, ginger, and lime.
The production of the traditional functional drink is commonly
conducted by extraction (Kamaruddin et al., 2017; Khairi &
Nurkhasanah, 2020). The extract from the process contains many
microorganisms and has a limited shelf life. This can pose challenges
during storage and transportation as the traditional functional drink is
perishable and can spoil quickly. Therefore, sterilization and concen-
tration of the traditional functional drink are important. The common
methods for sterilization and concentration are based on thermal pro-
cesses (Bozkir & Baysal, 2017). However, exposure to high tempera-
tures may degrade heat-sensitive bioactive compounds (Barba
et al., 2017). In addition, thermal sterilization may also not be effective
in eliminating all pathogens and contaminants, particularly those that
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MEUTIA ET AL.
are heat resistant. Membrane technology can be an alternative to
improve the quality of traditional functional drinks. Membrane tech-
nology has the advantages of being easy to operate, high energy effi-
ciency, environmentally safe, has a low energy consumption, and
simple as well as efficient membrane module (Liu et al., 2022).
Microfiltration (MF) is widely used for the removal of suspended
solids and is also applicable in the sterilization processes of liquid food
(Vieira et al., 2020). The advantages of processing functional drinks
with membrane technology are increasing juice yields, reducing the
use of enzymes, reducing waste products, and operating at low tem-
peratures to maintain their nutritional value (Conidi et al., 2017). In a
study using a ceramic membrane with a pore size of 0.2 μm, passion
fruit juice can be effectively clarified, even though a significant loss of
aroma was notably observed (Vaillant et al., 2001). Beer clarification
has been conducted using MF with pore size in the range of 0.2 and
0.65 μm. Superior products were obtained as the MF retained the col-
loids, particles, and yeast while passing through the solutes, salts, and
aromas (Cimini & Moresi, 2016; Freeman, 2015; Sman et al., 2012).
Sterilized and high-quality apple juice can be produced using ceramic
MF. Comparable taste and color to the fresh apple juice were
obtained, and the process is applicable in commercial production
(Harada et al., 2004). In coconut water processing, MF had been
proven to reduce turbidity and microorganism content. The sterilized
coconut water had a comparable total phenolic compound, soluble
solid, ions, and antioxidants to the fresh coconut water with an
extended shelf life of 30 days (Kailaku et al., 2017). However, the per-
meate flux declined by more than 90% during filtration due to aggra-
vating fouling (Karmakar & De, 2017). According to the result of the
study on TCM extract, the permeate produced by MF was lighter in
color and contained fewer precipitates. Removing foulant from the
feed to mitigate membrane fouling led to more efficient MF operation
(Wang et al., 2021). Results from the previous study emphasized the
applicability of MF as an alternative to the thermal-based clarification
and sterilization processes. However, the study of MF for
clarification and sterilization of traditional functional drinks is still
lacking.
Osmotic membrane distillation (OMD) is a non-isothermal separa-
tion process through hydrophobic membrane pores. In OMD, a feed
solution is circulated on one side of the hydrophobic membrane, while
a concentrated draw solution is circulated on the other side, generat-
ing vapor pressure as the driving force for water vapor transport from
the feed to permeate stream (Francis et al., 2022; Kujawski
et al., 2013). The draw solution should have high osmotic pressure,
neutral pH, be nontoxic, inert, and easy to regenerate (Wenten
et al., 2021). Several types of draw solutions that have been tested for
OMD are NaCl, Ca(NO3)2, polyethylene glycol, CaCl2, MgCl2 (Zhang
et al., 2021), sucrose, glucose, amino acids (Wenten et al., 2021),
K2CO3, K4P2O7 (Ongaratto et al., 2018). Even though CaCl2 is the
most commonly used draw solution for OMD, its application is limited
by the precipitation during the regeneration process. K4P2O7 does not
precipitate and produces solutions with identical osmotic potential to
CaCl2, making it an excellent alternative to CaCl2 (Ongaratto
et al., 2018). Furthermore, when K4P2O7 is utilized as a draw solution,

MEUTIA ET AL.
the losses of volatile compounds in liquid food can be minimized
(Alves & Coelhoso, 2006; Ongaratto et al., 2018).
OMD operates at lower temperatures and pressures than thermal
evaporation, hence resulting in significant energy savings and reduced
operating costs. In addition, the low operating temperature of OMD
leads to better preservation of nutrients, aroma, and taste of the con-
centrated products (Bhattacharjee et al., 2017). Juices such as kiwi
(Cassano et al., 2006), camu camu (Souza et al., 2013), cranberry
(Zambra et al., 2014), cactus pear (Terki et al., 2018), orange
(Ongaratto et al., 2018), pomegranate (Rehman et al., 2019) and apple
(Julian et al., 2020), have been concentrated by OMD with superior
nutrient preservation. However, low-permeate flux, fouling, and wet-
ting challenged the application of OMD (Julian et al., 2022). The con-
centration of TCM has been conducted by DCMD, which operation is
almost similar to the OMD, except for using water as the draw solu-
tion. However, the study focused on the effect of operating condi-
tions on permeate flux. The physicochemical properties, nutrient
content, antihyperglycemic activity, pH, and total dissolved solids
(TDS) of the concentrated TCM were not tested and discussed. Due
to the lack of OMD application in functional drink concentration,
more study is required to examine its applicability.
This research aimed to investigate the use of MF and OMD to
produce sterilized and concentrated traditional functional drinks
consisting of Java tea, sappan wood, C. xanthorrhiza, ginger, and lime.
The microbial rejection of MF was analyzed to verify the applicability
of MF in the sterilization process. The bioactive compounds of the
fresh and sterilized extracts were characterized to ensure that the
sterilized extracts still maintained the characteristics of functional
drinks. In the OMD process, the effect of operational parameters,
such as feed temperature and draw solution concentration, on the
flux profile and fouling deposition were investigated. To determine
the impact of OMD on the concentrated extracts quality, the total
phenolic compound, antioxidant activity, pH, and TDS were quanti-
tatively measured.
2 | M E TH O DO LO GY
2.1 | Materials
Java tea, sappan wood, C. xanthorrhiza, ginger, and lime were pur-
chased from the local market in Bandung, Indonesia. Folin–ciocalteu's
phenol reagents, gallic acid, and DPPH (1,1-diphenyl-2-picrylhydrazyl)
were purchased from Sigma Aldrich. Methanol was purchased from
Merck. Technical grade ethanol 70%-wt was purchased
from Onemed. All chemicals for characterization purposes were of
analytical grade. Membranes used in this study are commercially avail-
able hydrophobic Accurel polypropylene (PP) Q3/2 hollow fiber mem-
branes from Membrane GmbH, Germany, with a pore size of 0.2 μm,
a wall thickness of 200 μm, and an inner diameter of 600 μm. For the
MF process, the membranes were wetted by flowing 70%-wt ethanol
through the membrane pores for 5 min. The remaining ethanol was
then rinsed by deionized water prior to the extracts sterilization.
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3 of 15
2.2 | Extraction of traditional natural ingredients
The procedure for the extraction processes is referred to in the previ-
ous research (Mardhiyyah et al., 2019). Before the extraction, all
ingredients were rinsed in running water. Java tea and sappan wood
were put in separate filter clothes, then immersed in 1000 mL of
water at a temperature of ±95 C for 30 min. The extracts were col-
lected for further analysis. C. xanthorrhiza and ginger were blanched
using water at a temperature of ±95 C for 3 min. Afterward, the
C. xanthorrhiza and ginger were grated, put in separate filter clothes,
and then pressed to collect the extracts. The extracts were kept at
room temperature for ±18 h prior to analysis. The lime extract is
obtained by manually pressing the juice of the lime.
2.3 | Sterilization of extracts using microfiltration
The MF experiment set-up is shown in Figure 1 and operated with an
initial feed volume of 500 mL. Prior to the MF tests, the piping line
was sterilized by flowing 70%-wt ethanol for 5 min, followed by rins-
ing with deionized water to remove any trace of ethanol. The perme-
ability of the membrane used in MF test was 319 L/m2 h bar. The
feed pressure of all tests was set at 2 bar and the feed cross flow rate
was 0.32 m/s. The permeate volume was recorded every minute dur-
ing the test to obtain permeate flux profile. The operation was termi-
nated once the feed volume was reduced to 250 mL, which
represented a volume reduction factor (VRF) of 2. VRF is the ratio of
initial feed volume to the retentate feed volume and its value may
affect the MF retention to certain molecules. In this study, the VRF of
2 was selected as the permeate flux for all extracts was steady with-
out any dynamic changes, which indicated stable fouling rate. The per-
meate was analyzed for the total phenolic content, antihyperglycemic
activity, pH, TDS, antioxidant activity, and microorganism
concentration.
2.4 | Concentration of extract using osmotic
membrane distillation
The OMD tests were conducted in a submerged configuration, at
which the membranes were immersed in static feed solution, as
shown in Figure 1. The temperature of the feed was set constant
using a water bath. A peristaltic pump was used to circulate K4P2O7
draw solution in the membrane lumen at a flow rate 0.2 m/s. Perme-
ate volume was measured every 30 min during the test and the test
was terminated after 2 h of operation. In the study to identify opti-
mum operating conditions, a 50 mL of sterilized sappan wood extracts
was employed as the feed. The feed temperature was varied between
25 and 45 C, while the concentration of the draw solution was varied
at 550, 600, and 650 g/L. The temperature of the draw solution was
25 C for all tests. The optimum operating conditions were then
applied for the concentration process of other sterilized extracts. The
quantification of the total phenolic compound, antioxidant activity,

4 of 15
FIGURE 1 Microfiltration and osmotic membrane distillation experimental set-up. MD, membrane distillation.
pH, and TDS were conducted to indicate the quality of the concen-
trated extracts.
2.5 | Characterization
2.5.1 | Total phenolic contents
The total phenolic content of fresh, sterilized, and concentrated
extracts was determined by the Folin-Ciocalteau method. 1 mL of
sample and 5 mL of demineralized water were put in a vial. Then,
0.5 mL of the Folin-Ciocalteau reagent was stirred thoroughly into the
vial. The solution was incubated for 5 min in a dark room, added 1 mL
of Na2CO3 solution, and left for 1 h. A blank solution was prepared by
adding 10 mL of demineralized water, 0.4 mL of Folin-Ciocalteau, and
4 mL of 7.5% Na2CO3. The blank solution was left in a dark place for
1 h. The absorbance of the solution was measured using a UV–Vis
spectrophotometer at a wavelength of 725 nm. The measurements
were duplicated.
2.5.2 | Antioxidant activity
The antioxidant activity was tested following the DPPH method. A
2 mL acetate buffer pH 5.5, 3.75 mL of methanol, and 200 μL of
DPPH 0.1 mM were stirred to form a homogeneous solution. After-
ward, 50 μL of the sample was added, and the solution was incubated
 8
for 30 min at 37 C. After incubation, the absorbance was measured
using a UV–Vis spectrophotometer (Genesys 10) at a wavelength of
517 nm. The measurements were duplicated.
2.5.3 | Antihyperglycemic activity
The antihyperglycemic activity was measured following
α-glucosidase inhibition method described by Wijaya et al. (2018). The
analysis was performed using an Elisa reader (Biotek). A 10 μL of
the sample was mixed with 50 μL of 0.1 M phosphate buffer (pH 7.0),
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MEUTIA ET AL.
25 μL of 0.5 mM 4-nitrophenyl α-D-glucopyranoside, and 25 μL of
α-glucosidase solution (0.04 Unit/mL) in microplate wells. The solution
was incubated at 37 C for 30 min, and the reaction was terminated
by adding 100 μL of 0.2 M Na2CO3 solution. Blanks with enzymes
replaced by buffer were prepared to calibrate the background absor-
bance. Negative controls with samples replaced by methanol were
also prepared. Positive controls were prepared and contained acar-
bose (10 ppm). The measurements were conducted in two replicates.
2.5.4 | pH
pH measurement was conducted by using a pH meter (Mediatech
Generic Digital pH meter PH-009). The measurements were
duplicated.
2.5.5 | Total dissolved solid
Total dissolved solid was measured by a digital handheld TDS meter
and reported as ppm. The measurements were duplicated.
2.5.6 | Microorganism quantification
Microorganism quantification was performed by the total plate count
(TPC) method. A 1 mL sample to be tested was consecutively trans-
ferred into distilled water by a sterile pipette to reach up to 10 dilu-
tions. Then, 0.1 mL of the diluted sample was inoculated into the solid
agar medium. The samples were then incubated at 38 C for 2 days
prior to colony quantification.
2.5.7 | Foulant deposition on MF and OMD
the membrane
Scanning electron microscopy (SEM) at 1000 magnification was
used to evaluate the morphology of the deposited foulant on the MF

MEUTIA ET AL.
and OMD membrane surface. The composition of the foulants was
characterized by energy dispersive x-ray spectroscopy (EDS). Prior to
the characterization, the fouled membrane was rinsed in deionized
water and dried in ambient air for 24 h. The membrane samples were
sputtered with gold, and the characterizations were performed by a
Hitachi SU35000.
2.6 | Statistical analysis
The effect of sterilization by MF and concentration by OMD on
the total phenol, antioxidant activity, and antihyperglycemic activ-
ity of the extracts were evaluated using paired sample t-test with
a significance level of 0.05. The means of the total phenol, antioxi-
dant activity, and antihyperglycemic activity of the fresh extracts
were compared to that of the sterilized extracts after MF. A simi-
lar comparison was conducted for the sterilized extracts and con-
centrated extracts after the OMD operation. The optimum
2
operating conditions of OMD were identified by the flux. A 3 full
factorial design was used with feed temperature and draw solu-
tion concentration as the factors. The value of the low, medium,
and high levels of the feed temperature was 25, 35, and 45 C,
respectively. The value of low, medium, and high levels of the
draw solution concentration was 550, 600, and 650 g/L, respec-
tively. All tests were conducted in two replicates. Two-way analy-
sis of variance (ANOVA) was conducted to assess the overall
differences among the groups for feed temperature and draw
solution concentration, respectively. To determine which opera-
tion condition significantly resulted in different flux, Tukey's hon-
estly significant difference (HSD) test was conducted with a
significance level of 0.05. The residual plots for OMD flux were
analyzed to confirm that the data met the criteria of normal distri-
bution, linearity, and homoscedasticity.
3 | RESULT AND DISCUSSION
3.1 | MF performance for extracts sterilization
In this study, fresh extracts were clarified and sterilized by conducting
MF for each extract. The results suggested that the initial MF flux var-
ied depending on the type of feed solution. The ginger extract exhib-
ited the highest initial flux of 511 LMH, while the lime extract showed
the lowest initial flux of 58 LMH. This led to different operation times
to obtain the feed concentration factor of two. The flux declined over
time for all tests regardless of the type of extract. To investigate the
severity of the flux decline, the flux was expressed as normalized flux,
which accounts for the ratio of flux at a particular operation time (J) to
the initial flux of the test (J0) (Figure 2). In the MF process, fouling was
caused by large impurities such as starch, glucose, cellulose, and hemi-
cellulose contained in the fresh extracts. Flux reduction of 90%, 75%,
60%, 65%, and 64% was indicated for tests using C. xanthorrhiza,
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5 of 15
ginger, lime, Java tea, and sappan wood as the feed, respectively. In
MF tests of C. xanthorrhiza and ginger, rapid flux decline occurred in
the first 5 min of the operation. The lime sample experienced a sud-
den flux increase after 10 min of operation due to the occurrence of
the oil-in water emulsion.
The MF operation in this research was conducted in batch, at
which the retentate stream was recycled back to the feed tank. There-
fore, the concentration of extracts in the feed tank increased over
time as more permeate flowed through the membranes. This simulta-
neously led to more severe concentration polarization. Concentration
polarization refers to an increase in solute concentration adjacent to
the feed membrane interface due to permeate transfers through the
membrane pores and is an equilibrium process under a given set of
operating conditions. Solute accumulation becomes constant when
the concentration-driven rate of reverse diffusion to the bulk solution
equals the rate at which new solute is transported to the interface
through the bulk flow. The concentration polarization may lead to
increased mass transfer resistance due to a slower diffusion process
in the boundary layer compared to that in bulk solution. In addition,
severe concentration polarization increases the fouling propensity on
the membrane surface. Membrane fouling is an inevitable phenome-
non in membrane filtration, which reduces permeate flux due to pore
blocking. In tests using traditional extracts, the organic fouling was
aggravated due to the high concentration of organic substances in the
extracts, hence resulting in severe flux reduction. In addition, organic
fouling is common in hydrophobic membranes due to the lack of
hydration layers that can keep the adhesion of organic substances on
the membrane (Chang et al., 2020; Ding et al., 2008; Jafarinejad &
Esfahani, 2021; Johnson & Nguyen, 2017).
The visualization of the fresh and sterilized extracts is presented
in Figure 3. The fresh extracts of ginger and Curcuma xanthorriza
exhibited high turbidity due to the presence of organic impurities,
such as pectin, cellulose, hemicellulose, naringin, and terpenoids (Noor
et al., 2018), in the fresh extracts. The molecular size of pectin,
FIGURE 2 Profile of normalized flux of microfiltration test for
each extract.

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FIGURE 3 Visualization of the (a) fresh extracts (before microfiltration [MF]) and (b) sterilized extracts (after MF).
cellulose, and hemicellulose these compounds ranged from 400 to
5000 nm (Baker & Cameron, 1999) and are larger than the MF mem-
brane pores. The sterilized extract of ginger and Curcuma xanthorriza
were free of turbidity, emphasizing the clarification of extracts and
the retention of the impurities by MF, which suggest the increased
fouling propensity.
In MF test using lime extracts as the feed, 80% flux reduction
occurred in 60 min of operation. The fresh lime extract was turbid,
which may be due to the presence of pulp and fiber carried away dur-
ing the lime pressing. Carotenoid pigments, such as lutein and zeaxan-
thin, are also naturally present in lime and are responsible for the
yellowish color of the lime extract (Figure 3a). The sterilized lime
extract was visibly clear, as shown in Figure 3b. This indicates the
elimination of pulp, fiber, and carotenoid pigments by MF, which also
directly contributes to the flux decline. The retention of carotenoid by
MF was also reported by a previous study clarifying grapefruit juice
(Rouquié et al., 2019). In tests using Java tea and sappan wood
extracts, the flux decline was less severe than in the other extracts.
These are in agreement with the visualization of the extract's turbid-
ity. The Java tea and sappan wood extract has low turbidity compared
to the ginger, lime, and Curcuma xanthorriza extracts. No color change
was observed when comparing the fresh and sterilized sappan wood
extracts, while the yellowish color of the Java tea faded after the fil-
tration. The color change indicated the retention of flavonoid and tan-
nin, which are the yellow color contributing substances in Java tea.
The morphology of the membrane used in the MF operation using
Curcuma xanthorriza, ginger, and lime as the feed were analyzed with
SEM, while EDS was used to characterize the composition the fouling
layers. As shown in the SEM image of the pristine membrane, the
pores of the membrane are clearly visible (Figure 4a). However, on
the surface of the membrane used in tests using Curcuma xanthorriza,
ginger, and lime as the feed, most of the pores were blocked by the
fouling layer (Figure 4b–d, respectively). The EDS mapping indicates
that the fouling layers were composed of C, N, and O, which are the
elements of the organic impurities. The fouling on the membrane used
to sterilize Curcuma xanthorriza has formed a multi-layered foulant.
While the foulant had a porous structure when it was stacked, the
porosity of the fouling layer reduced significantly. In addition, the for-
mation of sharp and dense crystal structures was also observed in
many parts of the membrane. The permeate needed to pass through
the fouling layer, which provided additional mass transfer resistance.
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MEUTIA ET AL.
Hence, the permeate flux of the MF test using Curcuma xanthorriza as
the feed was significantly reduced by 90% of its initial flux. The foul-
ing layer might mostly consist of high molecular weight compounds,
such as terpenoids and pectin. In addition, the sharp crystal structure
observed in the SEM image suggested the deposition of curcumin-
based crystals, which are abundant in Curcuma xanthorriza.
In test to sterilize ginger extracts, the foulant deposited on the
membrane surface, forming a flaky structure which covered most of
the membrane pores. The foulant structure was uniform over the
entire membrane surface and might be consisted of starch, as one of
the most abundant components in ginger. Other components that
possibly deposited on the membrane surface were tannins, flavonoids,
and gingerol. In test to sterilize lime extracts, fouling deposition was
significant, however, many membrane pores were still clearly visible.
This supports the flux reduction data, which stated that only 50% of
flux reduction occurred during the MF of lime. The foulant was dense
with granulated structure that can consist of saponins, carotenoids,
and naringin from lime.
In the MF process, VRF of 2 was obtained by terminating the
tests once the feed volume was reduced by half. A membrane area of
0.0026 m2 was used. In an industrial-scale production treating 500 L
feed with a VRF of 2, a membrane area of 2.6 m2 is needed. In the
case that pre-treatment is not conducted and fouling occurs as
observed in this study, the operating time for the sterilization of Java
tea, sappan wood, ginger, lime, and C. xanthorrhiza is 40, 16, 20, 60,
and 60 min, respectively. To achieve more efficiency, the sterilization
process can be conducted at a higher VRF. Increasing the VRF to
4, while maintaining the membrane area of 2.6 m2 would lead to lon-
ger sterilization times, which are 69, 28, 42, 186, and 115 min for Java
tea, sappan wood, ginger, lime, and C. xanthorrhiza, respectively. The
extended sterilization time is due to the severe fouling that reduced
the MF permeate flux. This highlights the need for extracts pre-
treatment prior to MF and fouling mitigation strategy during the
MF. Fouling is the major drawback for sterilization of extracts by
MF. Mitigation should be done to improve the MF performance and
extend the operation time. Membrane cleaning is one of the most
applied strategy to remove the fouling from membrane surface, that
can be conducted physically, chemically, or biologically (Xiao
et al., 2023). Other strategies involves the optimization of filtration-
cleaning cycle, filtration duration, and physical flushing (Hube
et al., 2021).
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MEUTIA ET AL. 7 of 15

F I G U R E 4 Scanning electron
microscopic images and energy
dispersive x-ray spectroscopy
mapping of outer membrane surface:
(a) pristine membrane and after tests
using (b) Curcuma xanthorriza,
(c) ginger, and (d) lime as the feed
(purple, pink, and green dots in the
mapping represent carbon, nitrogen,
and oxygen, respectively).

3.2 | Quality analysis of the sterilized extracts
The quality of the sterilized extracts were characterized by determin-
ing the phenolic compound concentration, antioxidant activity, antihy-
perglycemic activity, pH, and TDS. The quality of the sterilized
extracts were then compared to the fresh extracts. The microbial anal-
ysis of the fresh and sterilized extracts are shown in Table 1. The
results signified the applicability of MF for the sterilization of the
extracts, as no colonies were identified in all sterilized extracts. The
pH value of the fresh and sterilized extracts was consistent, showing
the negligible effect of MF on the extract's acidity. Total dissolved
solids (TDS) are the amount of dissolved substances in water that may
affect the taste. Based on the data in Table 1, there are TDS reduction
in the sterilized extracts due to the filtration process.
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8 of 15 MEUTIA ET AL.

TABLE 1 Microorganism quantification, pH, and total dissolved solids (TDS) of the fresh and sterilized extracts.

Concentration (CFU/mL) pH TDS (ppm)

Sample Fresh Sterilized Fresh Sterilized Fresh Sterilized

Java tea 4.18  10 7
0 6.8 ± 0.00 6.8 ± 0.00 40 ± 4.24 40 ± 0.00
Sappan wood 1.31  10 8
0 6.6 ± 0.00 6.6 ± 0.00 197 ± 2.12 110 ± 2.83
Ginger 7.68  10 6
0 7.6 ± 0.64 6.2 ± 0.99 506 ± 2.12 262 ± 11.31
Lime 4.45  107 0 3.2 ± 1.63 3.2 ± 1.63 172 ± 4.24 104 ± 1.41
Curcuma xanthorrhiza 4.30  10 6
0 4.5 ± 0.28 4.5 ± 0.00 196 ± 6.36 168 ± 0.00

FIGURE 5 (a) Total phenol, (b) antioxidant activity, and (c) antihyperglycemic activity of the fresh and sterilized extracts.

The phenolic compound concentration of the fresh and sterilized
extracts are expressed as total phenol and shown in Figure 5a. The
fresh extract of Java tea showed the highest total phenol of 51.68
± 6.82 mg GAE/g extract, while C. xanthorrhiza had the lowest total
phenol of 5.20 ± 0.91 mg GAE/g extract. The reduction of total phe-
nol after MF operation was observed for all extracts. The statistical
analysis indicated a significant difference in the concentration of phe-
nolic compound between all fresh extracts and sterilized extracts. The
phenolic compounds in Sappan wood, Java tea, and ginger were
reduced by almost 40%, 24%, and 75% after MF, respectively. A sig-
nificant decrease in phenolic levels is an indication of the retention of
dominant bioactive compounds in the extract, for example, brazilein in
sappan wood extract, sinensetin in Java tea extract, and gingerol in
ginger. The antioxidant activity was reported as ppm AEAC and the
results are presented in Figure 5b. Among the fresh extracts, ginger
exhibited the highest antioxidant activity of 36 ppm AEAC. All steril-
ized extracts showed a statistically significant reduction of antioxidant
activity, however, ginger, lime, and C. xanthorrhiza extracts exhibited
the most prominent antioxidant activity reduction. A 72%, 30%, and
25% losses on the antioxidant activity were observed for ginger, lime,
and C. xanthorrhiza, respectively. As color is one of the attributes of
antioxidant activity, the severity of antioxidant activity reduction can
be characterized by observing the color change of the sterilized
extracts (Figure 3). While many researches have reported strong
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MEUTIA ET AL. 9 of 15

TABLE 2 Bioactive compounds in fresh extracts and the respective molecular weight.

Extracts Selected bioactive compounds in fresh extracts Molecular weight (Da) References
Sappan wood Brazilin 286.28 (A'yuni et al., 2022)
Java tea Sinensetin 372.40 (A'yuni et al., 2022; Febjislami et al., 2019)
Salvigenin 328.30
Ginger Gingerol 294.40 (Idris et al., 2019)
Shogaol 276.40
Paradol 278.40
Gingerdione 348.50
Lime Naringin 580.53 (Herawati et al., 2020)
Hesperidin 610.60
Curcuma xanthorrhiza Curcumin 368.40 (Badrunanto & Rafi, 2019)

correlation between the total phenolic concentration and antioxidant

activity in plant extracts (Aryal et al., 2019; Kumar et al., 2014;
Piluzza & Bullitta, 2011), in this study, only ginger extract showed a
correlation between the phenolic and antioxidant activity.
The total phenolic content of the sappan wood and java tea was
greatly reduced after MF, but the reduction of their antioxidant activ-
ity were not as drastic. In opposite, the reduction of total phenolic
compound of lime and C. xanthorrhiza were small (5.43% and 2.79%,
respectively) compared to the antioxidant activity (24.16% and
11.94%, respectively). This indicates the variation of bioactive com-
pounds in the extracts, at which the phenolic compounds could differ
from the antioxidant components. The antihyperglycemic activity of
the extracts was reported as % inhibition. High inhibition indicates the
ability of the extracts to inhibit the increase in blood glucose levels.
F I G U R E 6 Effect of feed temperature and draw solution
As presented in Figure 5c, sappan wood fresh extract obtained the
concentration on osmotic membrane distillation flux (tests were
highest % inhibition of 87%, and C. xanthorrhiza, fresh extract
conducted using sappan wood extract as the feed).
obtained the lowest % inhibition of 1.74%. According to the statistical
analysis, the antihyperglycemic activity of the sappan wood and
C. xanthorrhiza was significantly altered after MF. In contrast, no sig- a bigger molecular weight and size than that of MF MWCO. Some
nificant changes in antihyperglycemic activity were detected in the phenolic complexes, such as tannin-anthocyanin, anthocyanin–antho-
sterilized extracts of Java tea, lime, and ginger. cyanin, and tannin-proteins complexes, have been reported (Rayess
The separation process in MF occurs based on a sieving mecha- et al., 2011). The phenolic complexed formation can be the explana-
nism, wherein molecules larger than the membrane pore size are tion for lower phenolic compounds in sterilized extracts. Furthermore,
retained. However, information regarding the molecular size of the the reduction of phenolic compounds observed in the sterilized
bioactive compounds in the fresh extracts are limited and many refer- extracts could also be related to their adsorption on/in the membrane
ences mentioned the molecular weight of the compounds instead, as surface (Cassano et al., 2017). This hypothesis was supported by the
presented in Table 2. The MF membrane with a pore size of 0.1–1 μm SEM images (Figure 4), which showed substantial organic deposition
has a molecular weight cut-off (MWCO) of more than 100,000 Da on the membrane surface.
(Nguyen, 2012). As MWCO represents the weight of the molecules
that are 90% rejected by the membrane, this value might be used to
assess the rejection of bioactive compounds during MF. However, it is 3.3 | Effect of feed temperature and draw solution
worth noting that rejection of phenolic compounds in MF has been concentration on OMD flux
reported in previous studies, despite the lower molecular weight com-
pared to the MF MWCO (Magalhães et al., 2019; Rouquié Sappan wood extract was used as a feed to investigate the effect of
et al., 2019). The results suggested that the discussion regarding MF feed temperature and draw solution concentration on OMD flux due
rejection on phenolic compounds cannot be conducted by simply to its clarity and lower fouling propensity. All tests were conducted
comparing their molecular weight. The phenolic compound in the for 2 h, and the flux presented in Figure 6 are the average for each
fresh extracts might form complexes with other compounds that have test. The results indicated that OMD flux increases with the draw
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10 of 15 MEUTIA ET AL.

T A B L E 3 Honestly significant
Draw solution concentration (g/L)
difference test of osmotic membrane
Feed temperature ( C) 550 600 650 distillation flux at varied feed
temperature and draw solution
25 0.308 ± 0.06a,a 0.445 ± 0.008b,a 0.639 ± 0.09c,a
concentration.
35 0.378 ± 0.004a,b 0.636 ± 0.02b,b 0.748 ± 0.02c,b
a,b b,b
45 0.621 ± 0.07 0.744 ± 0.01 0.881 ± 0.06c,b

Note: Data with different letters for the same parameter are significantly different at a probability level of
0.05. The first and second letters indicated a comparison of the mean on the same row and column,
respectively.

solution concentration and feed temperature enhancement. As

describes by Antoine's equation, the water vapor pressure is a sub-
stantially rising function of temperature. Hence, at constant draw
solution temperature, the water vapor gradient increased with the
enhancement of feed temperature. Additionally, higher temperatures
reduce the viscosity of the feed, enhancing mass transfer
(Hongvaleerat et al., 2008; Ongaratto et al., 2018).
The concentration of K4P2O7 as a draw solution were varied at
550, 600, and 650 g/L. At similar feed temperatures, approximately
two-fold flux enhancement was observed when the draw solution
concentration increased from 550 to 650 g/L. Water forms bonds
with dissolved solids in liquids, preventing water from evaporating
and lowering the vapor pressure. With an increase in draw solution
concentration, the vapor pressure significantly decreases. Therefore,
low vapor pressure caused by high draw solution concentrations
results in a higher driving force to transport vapor to the draw solu-
tion stream.
The comparisons of means indicated that the OMD flux was sig-
nificantly affected by the draw solution concentration and feed tem-
perature. Further analysis by honestly significant difference test
indicated a clear difference in the OMD flux at increased draw solu-
tion concentration. The increase of feed temperature from 25 to 35 C
was also significantly affected the OMD flux. However, further feed
temperature enhancement to 45 C did not result in significant flux
change (Table 3). Higher feed temperature should result in increased
driving force. According to Raoult's Law, the vapor pressure of the
draw solution with concentration of 650 g/L was 3041 Pa. The vapor
pressure of feed at 25, 35, and 45 C was 3166, 5620, and 9580 Pa,
respectively. The driving force for mass transfer then can be deter-
mined by calculating the difference between the feed vapor pressure
F I G U R E 7 Profile of (a) flux and (b) normalized flux of osmotic
and draw solution vapor pressure. The diving force was 125, 2579,
membrane distillation tests for each extract.
and 6539 Pa for OMD at feed temperatures of 25, 35, and 45 C,
respectively. As OMD flux is a linear function of driving force, the
results indicated an exponential increase of flux when the feed tem- the temperature to 45 C had a negligible impact on the flux, but it
perature increased. The experimental data, however, showed only might adversely affect the bioactive compounds in the extracts and
15.7% and 31.7% flux enhancement when the feed temperature was necessitated a higher amount of thermal energy.

raised to 35 and 45 C, respectively. The deviation was due to the
occurrence of temperature polarization, which becomes more severe
at operation of higher feed temperature. Based on the result, the 3.4 | OMD performance for concentrated extracts
selected draw solution concentration for the OMD operation is
650 g/L as it produced the highest flux, hence, reducing the time In OMD, the extracts were concentrated to increase the concentra-
required for the concentration process. Meanwhile, a feed tempera- tion of the active compounds. The profile of OMD flux is shown in
ture of 35 C was selected as it produced moderately high flux. Raising Figure 7a. The results suggested that the initial OMD flux varied

MEUTIA ET AL.
TABLE 4 Concentration factor, pH, and TDS of functional drink ingredients after OMD.
pH
Sample Concentration factor Sterilized
Java tea 1.24 6.8 ± 0.00
Sappan wood 1.24 6.6 ± 0.07
Ginger 1.15 6.2 ± 0.99
Lime 1.13 3.2 ± 0.14
Curcuma xanthorrhiza 1.10 4.5 ± 0.00
Abbreviations: OMD, osmotic membrane distillation; TDS, total dissolved solids.
depending on the type of feed solution. The Java tea extract exhibited
the highest initial flux of 1.07 LMH, while the C. xanthorrhiza extract
showed the lowest initial flux of 0.52 LMH. This is in accordance with
the TDS of the feed (Table 4), as Java tea had a low TDS and
C. xanthorrhiza had a high TDS. The test using sappan wood as the
feed exhibited the most stable flux. The gradual flux reduction was
observed at all tests and the severity of the flux reduction was con-
veyed by the normalized flux profile (Figure 7b). The reduction of the
normalized flux was 67% (ginger), 65% (lime), 45% (C. xanthorrhiza),
20% (Java tea), and 5% (sappan wood). The OMD performance is
quantified by the concentration factor (CF), which is the ratio of the
initial and final feed volume. The CF of tests using ginger, lime,
C. xanthorrhiza, Java tea, and sappan wood as the feed was 1.15, 1.13,
1.10, 1.24, and 1.24, respectively. In this study, the OMD operation
time was limited to 2 h, to prevent bioactive degradation due to the
excessive exposure to heat and oxygen. To achieve much higher CF,
OMD module with a higher membrane area by increasing the number
of membranes, can be an alternative strategy.
The flux decline in OMD operation occurs due to the decreasing
driving force, which is the vapor pressure gradient between the feed
and draw solution. Over time, more vapor pressure is transported
from the feed solution to the draw solution, resulting in the increased
concentration of the feed and reduced concentration of the draw
solution. The direct consequence of vapor transport is the lower and
higher vapor pressure on the feed side and draw solution stream,
respectively. This leads to the reduction of the driving force for vapor
transport. In addition, the increase feed concentration may induce
fouling that reduces the active surface area and permeate flux. To
investigate the fouling deposition, the outer membrane surface after
OMD tests using C. xanthorrhiza, ginger, and lime as the feed were
characterized (Figure 8a–c, respectively). Patchy foulant deposition
was observed on the membrane surface. However, most of the mem-
brane pores were still clearly visible. As the flux reduction of tests
using C. xanthorrhiza, ginger, and lime were close to or more than
50%, fouling was not the main cause. As the OMD operation con-
tinues, the feed concentration gradually increases, that resulted in the
reduction of driving force and permeate flux. Fouling, however, was
still inevitable and need to be further addressed. In MD studies, foul-
ing mitigation by modifying the membrane structure and materials has
shown great potential. Superhydrophobic membrane, which has lower
surface energy than hydrophobic membrane possessed superior
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11 of 15
TDS (ppm)
Concentrated Sterilized Concentrated
6.7 ± 0.00 40 ± 0.00 40 ± 0.00
6.5 ± 0.07 110 ± 2.83 109 ± 0.00
4.9 ± 0.14 262 ± 11.31 254 ± 0.00
3.4 ± 0.14 104 ± 1.41 102 ± 0.00
4.4 ± 0.00 168 ± 0.00 164 ± 0.00
fouling resistance (Lin et al., 2015; Warsinger et al., 2015). Further
improvement involves the application of omniphobic material, which
also applicable for feed containing oily substances (Goh et al., 2013;
Hausmann et al., 2013). Janus membrane, which combines materials
of opposing wettability, has been proved to prevent the adsorption of
nonpolar substances, hence avoid fouling formation (Guillen-Burrieza
et al., 2016; Rezaei et al., 2018). Further study on the application of
novel OMD membrane for concentration of extracts should be con-
ducted for improved performance.
3.5 | Quality analysis of concentrated extract
The quality of the concentrated extracts was characterized by mea-
suring the phenolic compound concentration, antioxidant activity,
pH, and TDS. The quality of the concentrated extracts were then
compared to the sterilized extract. The phenolic compounds of ster-
ilized and concentrated extracts are shown in Figure 9a. The
sterilized extract of Java tea showed the highest total phenol of
39.85 ± 1.89 mg GAE/g extract, while C. xanthorrhiza had the low-
est total phenol of 5.95 ± 0.91 mg GAE/g extract. The phenolic
compounds in all concentrated extracts were higher than in their
respective fresh extracts. However, the direct measurement of the
phenolic compounds in the concentrated extracts needs to be care-
fully interpreted. The increase in the measured phenolic compounds
concentration may occur due to the reduction of water as a solvent
in the extracts. To further investigate the preservation of active
compounds in the concentrated extracts, the measurement of phe-
nolic compounds concentration should be conducted considering
the concentration factor of the process. The phenolic compounds
concentration in the concentrated extracts that were calculated in
regards to the concentration factor is shown in Figure 9a and
labeled as concentrated extracts-CF. Even though the statistical
analysis indicated a significant reduction in the phenolic compounds
concentration of Java tea, sappan wood, ginger, and lime after
OMD concentration, the %reduction were relatively minor. The
phenolic compounds concentration of concentrated Java tea and
sappan wood were reduced by 7% and 13%, respectively, compared
to the sterilized extracts. While those of ginger and lime were 22%
and 5%, respectively. Even though the statistical analysis indicated
a significant reduction of the phenolic compounds concentration of
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12 of 15 MEUTIA ET AL.

F I G U R E 8 Scanning electron
microscopic images and energy dispersive
x-ray spectroscopy mapping of outer
membrane surface after tests using
osmotic membrane distillation (a) Curcuma
xanthorrhiza, (b) ginger, and (c) lime as the
feed (purple, pink, and green dots in the
mapping represent carbon, nitrogen, and
oxygen, respectively).

FIGURE 9 (a) Total phenol and (b) antioxidant of the sterilized and concentrated extracts.

Java tea, sappan wood, lime, and C. xanthorrhiza after OMD concen- sterilized extracts. While those of lime and C. xanthorrhiza were 5%
tration, the % reduction were relatively minor. The phenolic com- and 3%, respectively.
pounds concentration of concentrated Java tea and sappan wood The antioxidant activity results are presented in Figure 9b. All
were reduced by 7% and 13%, respectively, compared to the concentrated extracts showed increased antioxidant activity due to

MEUTIA ET AL.
the retention of the active compounds in OMD operation. Antioxidant
activity enhancement of concentrated extracts occurred due to OMD
concentrating process. Similar to the phenolic compounds concentra-
tion, the antioxidant activity of the concentrated extracts should be
calculated, taking into account the concentration factor of the feed.
The statistical analysis showed a significant reduction in antioxidant
activity among the concentrated extracts of Java tea, sappan wood,
ginger, and lime. However, C. xanthorrhiza did not have a significant
impact on the reduction of antioxidant activity. The decrease in anti-
oxidant activity of 5.95%, 7.02%, 12.05%, 24.16%, and 11.94% was
indicated in sappan wood, Java tea, ginger, lime, and Curcuma xanthor-
riza, respectively. As mentioned in Table 4, the pH and TDS values of
the sterilized and concentrated extracts were consistent, showing the
negligible effect of OMD. The quality analysis of the concentrated
extracts highlights the outstanding ability of OMD to preserve the
active compounds and maintain the physicochemical properties of tra-
ditional functional drink ingredients.
4 | C O N CL U S I O N
Traditional functional drinks consist of C. xanthorrhiza, ginger, lime,
Java tea, and sappan wood extracts are can be sterilized and concen-
trated using membrane-based nonthermal technology. MF showed
superior performance in sterilizing all extracts, indicated by the
absence of colonies in total plate count characterization. MF can also
remove turbidity from extracts, resulting in less TDS and visually clear
extracts. However, the sterilization process using MF leads to a
decrease in total phenolics and antioxidant activity of the extracts due
to the conservation of certain active compounds. Similarly, the antihy-
perglycemic properties of sappan wood and ginger also decline. The
reduction overall in phenolic content, antioxidant activity, and antihy-
perglycemic effects is determined by the MWCO of the membrane.
Despite the small size of phenolic compounds, they can combine with
other compounds to form complex substances and adsorb on/in the
membrane surface, leading to diminished values in the permeate.
The OMD flux were affected by feed temperature and K4P2O7
draw solution concentration. However, when the feed temperature
increased from 35 to 45 C, there was no significant increase in flux.
Therefore, OMD experiments were conducted at a feed temperature
of 35 C to reduce thermally-induced nutrient degradation. The con-
centration factors of 1.15, 1.13, 1.10, 1.24, and 1.24 were obtained
for ginger, lime, C. xanthorrhiza, Java tea, and sappan wood, respec-
tively. The OMD flux decreased over time despite negligible foulant
deposition, emphasizing the reduction of driving force during opera-
tion. In the concentrated extracts, the bioactive compounds were
effectively preserved, with minor decline on the phenolic concentra-
tion and antioxidant activity Therefore, OMD can still be regarded as
effective in preserving the bioactive content.
AUTHOR CONTRIBUTIONS
Fahliza Meutia: Data curation, formal analysis, investigation, method-
ology, writing-original draft, writing – review and editing. C. Hanny
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13 of 15
Wijaya: conceptualization, methodology, supervision, writing – review
and editing. Helen Julian: conceptualization, funding acquisition,
methodology, resource, supervision, writing review and editing.
ACKNOWLEDG MENTS
The authors gratefully acknowledged the financial support from Pene-
litian, Pengabdian kepada Masyarakat, dan Inovasi (PPMI) 2022 Insti-
tut Teknologi Bandung.
CONFLIC T OF INTER E ST STATEMENT
The authors declare no conflicts of interest.
DATA AVAILABILITY STAT EMEN T
The data that support the findings of this study are available from the
corresponding author upon reasonable request.
OR CID
Helen Julian https://orcid.org/0000-0002-6698-0553
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How to cite this article: Meutia, F., Wijaya, C. H., & Julian, H.
(2023). A novel approach for sterilization and concentration of
traditional functional drinks: Membrane-based nonthermal
processes. Journal of Food Process Engineering, 46(12), e14479.
https://doi.org/10.1111/jfpe.14479