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Effect of different drying methods on the morphological structure, colour profile

and citral concentration of Lemongrass (Cymbopogon citratus) powder

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 Asian J Agric & Biol. 2019;7(1): 93-102.
AJAB Original Article

Effect of different drying methods on the morphological structure, colour

profile and citral concentration of Lemongrass (Cymbopogon citratus)
powder
Muhamad Asri Hashim1, Faridah Yahya1*, Wan Aida Wan Mustapha2
1
School of Food Science and Technology, Universiti Malaysia Terengganu (UMT), Kuala Nerus, Terengganu, Malaysia
2
School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia
(UKM), Bangi, Selangor, Malaysia
Received:
September 29, 2018 Abstract
Accepted: Lemongrass is a well-known aromatic herb due to its strong lemony odour which
January 31, 2019 contributes to several volatile compounds such as citral, β–myrcene and limonene.
Published: Volatile compounds of the aromatic herb are consequently difficult to restrain due to
March 30, 2019
high volatility and adverse effect caused by thermal treatment applied during
processing. Therefore, this study was conducted to determine the effect of different
drying methods on the morphological structure, colour profile and citral concentration
of lemongrass powder. Lemongrass powder was prepared by drying the fresh
lemongrass stalks with oven drying, vacuum drying and freeze-drying. The yield of
lemongrass powder resulted after drying processes were in the range of 9.92-11.09%.
The morphology structures of all lemongrass powders were flake-like structure,
irregular size, shrunk and appeared of pores. The freeze-dried powder was brighter in
colour with L* value of 84.51 ± 1.64 and obtained the highest citral concentration of
321.41 ± 19.97 ppm. This study suggested that freeze-drying was the suitable method
for preserving the colour qualities and citral compound of lemongrass powder. The
freeze-dried powder of lemongrass has high potential to be applied in the food and
beverage products.

Keywords: Lemongrass, Freeze dried powder, Drying methods, Colour profile,

Citral concentration

How to cite this:

Hashim MA, Yahya F and Mustapha WAW, 2019. Effect of different drying methods
*Corresponding author email: on the morphological structure, colour profile and citral concentration of lemongrass
[email protected] (Cymbopogon citratus) powder. Asian J. Agric. Biol. 7(1): 93-102.
This is an Open Access article distributed under the terms of the Creative Commons Attribution 3.0 License.
(https://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium,
provided the original work is properly cited.

Introduction India (Francisco et al., 2011). Volatile composition of

lemongrass was dominated by citral compound; a
Lemongrass is a local perennial grass plant known for combination between two geometric isomers; neral
the strong lemony odour which comes from Poaceae and geranial which contributed to the lemony odour
family that grows in tropical and subtropical climate (Pengelly, 2004). According to Bassolé et al. (2011),
countries such as Southeast Asia including Indochina, neral and geranial consist of 34.6% and 48.1%
Indonesia, Malaysia, Sri Lanka, North and Southern respectively of the total volatile composition of

Asian J Agric & Biol. 2019;7(1):93-102. 93

Muhamad Asri Hashim al
lemongrass. In addition, Skaria et al. (2012) stated that Material and Methods
aroma of lemongrass also contributed by myrcene
(12.75%), geranyl acetate (3.0%), methyl heptanene The standard of citral compound (assigned as 99.8%
(2.62%), geraniol (1.85%) and β- elemene (1.33%). purity) was purchased from Sigma-Aldrich Co.
Previously, parts of lemongrass have been used in (Malaysia). Fresh lemongrass stalks were purchased
traditional folk medicine for treating nervous and from a local market in Kuala Nerus, Terengganu,
gastrointestinal disturbance and as antispasmodic, Malaysia.
analgesic, anti-inflammatory, antipyretic, diuretic and
sedative (Santin et al., 2009). Lemongrasses are also Preparation of lemongrass powder
commonly used in food flavouring (Katsukawa et al., Fresh lemongrass stalks with moisture content of 80.0
2010), fragrance (Katsukawa et al., 2010), ± 5.0% (w. b) were cleaned and rinsed using tap water
pharmaceutical (Shah et al., 2011), and cosmetic to remove dirt and dust prior to cut into 16 cm lengths
(Mohamed Hanaa et al., 2012) industry. and chopped into small pieces. The sample was then
Drying and powdering techniques were recommended divided into three dried portions. Each portion (300.0
for preserving and improving the qualities of the ± 5.0 g) was dried using three drying methods i.e. oven
product purposes such as extending the shelf-life drying, vacuum drying and freeze drying.
(Dirim and Caliskan, 2012), inhibiting of product’s For oven drying, the sample was spread evenly on an
spoilage, minimizing thermal stress as well as aluminium foil on the oven dryer tray. Then, it was
retaining aroma compounds (Hossain et al., 2010; dried at 60.0 ± 2.0oC for 24 h in a conventional oven
Kubra and Rao, 2012; Dirim and Caliskan, 2012). dryer (UFB 500, Memmert, Germany). The second
Drying methods were significant effected the portion of the sample was dried using vacuum-pump
characteristics of dried product in term of oven dryer (ADP-21, Yamato, Japan) under drying
microstructure (An et al., 2016; Gasmalla et al., 2017), temperature of 60.0 ± 2.0oC for 24 h. The third portion
colour profile (Nikjooy and Hashemi, 2014) and of the sample was frozen in the freezer (MDF-U55V-
volatile composition (Díaz – Maroto et al., 2002; PE, Panasonic, Japan) for 24 h at - 80 ± 2.0oC prior to
Mohamad Hanaa et al., 2012). Studies have been done freeze drying process at - 47.0 ± 2.0oC. The heating
on the effect of drying method such as oven drying plate of freeze dryer was automated to 20.0 ± 3.0oC on
(Mohamed Hanaa et al., 2012; Pirbalouti et al., 2013), vacuum degree at 0.203 kPa.
freeze drying (Díaz – Maroto et al., 2002; Tajidin et After all the drying processes ended, the dried
al., 2012) and vacuum drying (Kruma et al., 2011) on lemongrass was ground into powder form for 30 s by
fresh herbs such as parsley (Díaz – Maroto et al., using mill grinder (IKA® Werke Staufen - MF 10.21,
2002), Pandan leaves (Yahya et al., 2010) and Germany) prior to storage at 4.0 ± 1.0oC in zipping
lemongrass (Mohamad Hanaa et al., 2012). During lock polyethylene bag prior to further analysis.
oven drying process, aroma preservation should take
into consideration as a challenge due to volatile Determination of total yield of lemongrass powder
susceptibility which may contributed by high Sieving analysis was carried out on modified method
temperature used and prolong exposure to the heat from Capariño et al. (2012) by stacking and vibrating
(Nawirska et al., 2009). Meanwhile, vacuum drying the sieve on the sieve shaker (Retsch Model AS 200
caused a minimal shrinkage on the structure of product digit, Germany) with test sieve (size of 250 μm) at the
(Alibas, 2007; Alibas, 2009) as well as inhibited amplitude of 60 for 20 min. Then, sieved samples
pigment degradation and nonenzymatic reaction were collected, and the final weight was recorded. The
(Methakhup et al., 2005; Alibas, 2007). Whereas, total yield of lemongrass powder was calculated by
freeze-dried product exhibited similar colour profile the following equation:
with the fresh ones such as on Goldenberry Total yield of lemongrass powder (%) =
(Valdenegro et al., 2013) and retained a greater
concentration of aroma compounds of parsley (Díaz – Weight of sieved powder (g)
Maroto et al., 2002). Therefore, the purpose of this × 100
Initial weight of chopped lemongrass stalk (g)
research was to determine the effect of different drying
methods on the morphological structure, colour profile
and citral concentration of lemongrass powder.

Asian J Agric & Biol. 2019;7(1):93-102. 94

Muhamad Asri Hashim al
Determination of moisture content surrounding the vial. Extraction of citral compound
A 2.0 ± 0.5 g of lemongrass powder were weighed into was conducted at 60.0 ± 2.0oC for 30 min by using
the crucible. The sample was dried using oven drying carboxen/ polydimethylsiloxane (CAR/PDMS) fibre.
method (AOAC, 2000) in the conventional oven CAR/PDMS fibre was then immediately inserted into
(BINDER, ED400, Germany) at 105 ± 2.0oC for 24 h. the injection port of the gas chromatography (GC
Moisture content of lemongrass powder was 2010 - Shimadzu, Japan) for 5 min at 250oC. Gas
determined by the equation below; chromatography-flame ionization detector (GC –
Percentage of moisture content (%) = FID) analyses were carried out by GC 2010
(Shimadzu, Japan) within operation started at 60oC,
Weight of powder before drying (g) - Weight of powder after drying (g)
× 100 increased 4oC/min to 150oC, then to 250oC at
Weight of powder before drying (g)
20oC/min and equilibrium for 5 min. A BPX-5
Determination of colour profile capillary column (30 m × 0.25 mm internal diameter,
The colour profile of the lemongrass powder was 0.25 μm film thickness) was used in this analysis. The
determined by using Minolta CR300 chroma meter chromatographic conditions were as follows: helium
(Konica-Minolta, Japan) in term of L*, a* and b* (carrier gas) flow at 30.0 ml/min, the temperature of
values in triplicate analyses as adapted method from the injector at 250oC, temperature detector at 250oC
Arslan and Özcan, (2008). It was calibrated by using with pressure of 100 kPa.
a standard calibration with a white tile. A 25.0 ± 1.0 g The extraction of citral compound of the lemongrass
of lemongrass powder was packed in the zip-lock powders were performed by similar procedure used
polyethylene bag. The chromameter was put directly for standard solution. Fresh lemongrass was used as a
on the packed of lemongrass powder. control. The two isomers of citral; neral and geranial,
were identified by comparing retention times to
Determination of morphology structure authentic standards. While concentration of citral
The morphology structure of lemongrass powder was compound was expressed as the sum of concentration
observed under Scanning Electron Microscope (JEOL of neral and geranial obtained from separated standard
JSM – 6360, Japan) as adapted from Tonon et al. curve (concentration vs peak area).
(2008) to identify the differences occurred by different
drying methods. It was coated with 3.5 mA Statistical analysis
gold/palladium under vacuum condition by using auto Data of samples were analyzed using MINITAB 14
fine coater (JEOL JFC – 1600, Japan). Then, it was software (MINITAB Inc., State College, PA, USA) at
examined and operated at an accelerating voltage of p < 0.05. The one-way analysis of variance (One – way
5kV under 300× magnification. ANOVA) was used to determine the differences
between mean values of samples, followed by Fisher’s
Identification and quantification of citral Least Significant Difference (LSD) test to determine
concentration the significant differences among samples.
Quantitative analysis of citral compound of standard
solution were performed as method modified from Results and Discussion
Pellati et al. (2005) by headspace–solid phase
microextraction (HS-SPME) accompanied by gas Total yield of lemongrass powder
chromatography-flame ionization detector (GC-FID). Table 1 shows the total yield of powder, moisture
Stock solution of citral compound (20.0 ± 0.05 ml of content and colour profile of lemongrass powders
1000 ppm) was prepared by diluted the standard prepared by different drying methods. As can be seen
compound with distilled water. Then, the stock in Table 1, the total yield of lemongrass powders from
solution was diluted with another distilled water for different drying methods were in the range of 9.92-
preparing 20 ml of the standard solution of citral 11.09% and the oven drying produced higher yield of
compound with series of concentrations of 25, 50, 75, lemongrass powder compared to other drying
100 and 125 ppm. conditions. This result was in contrast with studies
The standard solution of citral compound (1.0 ± 0.05 done by Kim et al. (2006) and Lee et al. (2012a) on
ml) was measured in 45 ml of headspace vial. Heating Citrus "Hallabong" in which the author and co-
block was heated to equilibrate the temperature workers reported that a higher yield of powder
obtained by freeze-dried sample (20.0-22.5%) when

Asian J Agric & Biol. 2019;7(1):93-102. 95

Muhamad Asri Hashim al
compared to oven dried ones (17.5-22.0%). This study followed by freeze-dried and the oven-dried powder
also found that the total yield of freeze-dried was with 9.44 ± 0.29% and 8.66 ± 1.03% of moisture
higher when compared to vacuum-dried powder and content respectively (Table 1). It was in good
this result was in good agreement with study done by agreement with study done by Wijewardane et al.,
Rabeta and Lai, (2013) on total yield of Ocimum (2015) on dried pumpkin but in contrast with Neoh et
tenuiflorum powder. However, the total yields of al., (2016) who reported that the moisture content of
lemongrass powder were not significantly affected freeze dried red seaweed was higher (11.19%)
(p>0.05) by different drying methods (Table 1). As compared to oven dried (10.41%) and vacuum dried
expected, similar drying temperature of oven drying (10.31%) ones. According to Yousif et al., (1999) and
and vacuum drying at 60oC as well as constant in Artnaseaw et al., (2010) drying temperature and time
particle size of powder (250 µm) might cause an were affected the rate of water evaporation during
insignificant result of the yield of lemongrass powder. moisture removal on the heat transfer into the interior
of the material. Therefore, no significant effect was
Moisture content of lemongrass powder observed on moisture content of oven dried and
Moisture content of lemongrass powders from vacuum dried lemongrass powder in where both
different drying methods is shown in Table 1. The methods use the same temperature of 60°C as
moisture content of all lemongrass powders and fresh previously reported by Arslan and Özcan, (2010) on
lemongrass were determined by oven drying at 105oC Allium cepa. L.
for 24 h. As can be seen, the moisture content of fresh
lemongrass was 88.54 ± 3.08% while the moisture Colour profile of lemongrass powders
content of lemongrass powders was ranged from 8.64- There was a significant difference (p<0.05) of the
10.26%. As expected, the fresh lemongrass was colour profile of lemongrass powder between
experienced water removal up to 88% during the different drying methods. Freeze-dried lemongrass
dehydration process. It was typical for the fresh plant powder exhibited the highest L* value with lower a*
had up to 80% of water removal as it was in good and b* values as compared to oven-dried and vacuum-
agreement with study done by Carpenter and dried lemongrass powders. It is because of usage of
Carpenter, (2015) who reported that in the range 50- low drying temperature that prevented the enzymatic
90% of moisture content in fresh plants was lost browning to be occurred (Krokida and Maroulis,
during dehydration. This result also in line with 80% 2000), thus produced brighter colour of powder. The
of water removal from fresh pandan leaves after freeze-dried lemongrass powder obtained similar
drying processes (Yahya et al., 2010). effect on the L* value with various freeze-dried
The different drying methods were not significant powders from previous studies such as on mango
influenced (p>0.05) on the moisture content of (Capariño et al., 2012), Citrus "Hallabong" (Lee et al.,
lemongrass powder. But, vacuum-dried powder 2012a), chilli (Toontom et al., 2012) and apple (Antal,
showed high in moisture content (10.26 ± 1.39%) 2015).

Table 1: Physical properties (n=3) of lemongrass powders from different drying methods

Colour profile
Lemongrass Total yield of Moisture
powder powder (%) content (%)
L* a* b*
Control
- 88.54 ± 3.08a - - -
(fresh)
Oven dried 11.09 ± 1.33a 8.66 ± 1.03b 74.57 ± 1.73b 5.31 ± 0.38a 20.76 ± 1.74a

Vacuum dried 9.92 ± 0.94a 10.26 ± 1.39b 76.05 ± 2.66b 2.62 ± 1.78b 22.41 ± 0.73a

Freeze dried 10.81 ± 1.15a 9.44 ± 0.29b 84.51 ± 1.64a -1.14 ± 0.65c 17.89 ± 0.91b
Mean values with different superscript letters in the same column are significantly different at p<0.05.

Asian J Agric & Biol. 2019;7(1):93-102. 96

Muhamad Asri Hashim al
Nevertheless, the L* values on oven-dried and structure was performed. The structure of oven dried
vacuum-dried lemongrass were insignificantly (Figure 1a) and vacuum dried (Figure 1b) of
(p>0.05) affected by the drying methods (Table 1). It lemongrass powder were heat-dried Shiitake
is due to low heating temperature applied (60oC) mushroom-like structure studied by Tian et al. (2016).
during dehydration process which may inhibits According to Lee et al. (2012b), wrinkles were formed
Maillard reaction and non-enzymatic reaction from on the dried structure due to the increasing of drying
occurred (Artnaseaw et al., 2010). Table 1 also shows temperature which promotes an increase of moisture
the highest a* value and b* value of lemongrass stress and drying rate. Apart from that, vacuum drying
powder were obtained from oven drying (5.31 ± 0.38) technique caused the formation of small channels on
and vacuum drying (22.41 ± 0.73) treatment, side of the lemongrass powder. The vacuum condition
respectively. According to Maskan, (2001), was allowed rapid moisture transfer to the
chlorophyll and non-enzymatic reaction are surrounding area by creating high vapour pressure
responsible for the alteration of the colour profile of between the product and the drying chamber and
a* and b*. Therefore, these results may contribute by causing the cell to swell and formed large channels
loss of green colour due to the degradation of inside the sample (Kantrong et al., 2014; Tian et al.
chlorophyll pigments during drying process (Guiné 2016).
and Barroca, 2012; Sledz and Witrowa – Rajchert, Furthermore, the freeze-dried lemongrass powder
2012) which may lead to cause another pigment such appeared a skeletal-like structure with slightly smooth
as carotenoid becomes more visible (Sledz and and flaky with large porous (circled structure of
Witrowa – Rajchert, 2012). Figure 1c). The microstructure of freeze-dried
lemongrass was similar with porous structure on the
Morphology structure of lemongrass powders freeze-dried button mushroom as studied by
The morphological structure of oven-dried, vacuum- Argyropoulos et al., (2011). Freeze-dried lemongrass
dried and freeze-dried lemongrass powder is shown in powder experienced less breakage due to the
Figure 1. The structure of oven-dried lemongrass protection effect provided by ice crystals those
powder was observed to be flake, appeared more surrounding the material which was developed during
shrinkage and collapsed of cellular tissue (Figure 1a). freezing (-80oC) prior to drying in the chamber as
The pointy - edge of small particles with irregular explained by Ratti, (2001).

Powder Oven dried Vacuum dried Freeze dried

(a) (b) (c)

Lemongr
ass
powder

Fig. 1. Scanning electron microgram of lemongrass powders from different drying methods at 300×
magnification (red circle indicated the changes of the microstructure of lemongrass powder)

Asian J Agric & Biol. 2019;7(1):93-102. 97

Muhamad Asri Hashim al
Citral concentration of lemongrass powders The unknown peaks were detected during qualitative
The gas chromatogram of standard citral compound, analysis which indicated that lemongrass is composed
citral from fresh lemongrass and citral from of various aroma compounds such as linalool, β-
lemongrass powders were shown in Figure 2a, Figure myrcene, caryophyllene, citronellol, juniper camphor
2b and 2c-e, respectively. The isomers of citral and geranyl acetate as identified by Tajidin et al.,
compound; neral and geranial were detected at (2012). The unknown peaks also showed with
retention time 14.9 min and 16.0 min, respectively. different levels of peak height. As can be seen in
Various peaks were detected after peak detection of Figure 2b, the unknown peaks of fresh lemongrass
neral and geranial of fresh lemongrass (Figure 2b). showed higher peak height when compared to height
of unknown peaks of lemongrass powders (Figure 2c-
(A) (1) (2) e). This observation also indicated that volatile
compound of lemongrass had greater of peak height
from unknown peaks those detected from oven dried
and vacuum dried powder when compared to peak
height of freeze dried ones.
Figure 3 showed the citral concentration of
lemongrass powders from different drying methods. It
showed that citral concentration of lemongrass
powders was significantly affected (p<0.05) by
(B) (2)
(1) different drying methods applied. The citral
concentration of fresh lemongrass was 97.75 ± 7.29
ppm. The range of citral concentration of lemongrass
powders was 123.13 – 321.41 ppm. The fresh
lemongrass exhibited lower of citral concentration
compared to citral concentration of all lemongrass
powders. This result was contradicted with volatile
(C) (2)
composition of other fresh plant (Díaz-Maroto et al.,
(1)
2002; Calín-Sánchez et al., 2011). This situation
happened because of heat temperature and extraction
time of headspace solid phase micro-extraction
applied in this study were weak to give affect the
parenchyma layer and biological structure of the oil
(2) glands for citral to evacuate out during extraction of
(D) (1) fresh ones. Lewinsohn et al. (1998) found that isomers
of citral compound on fresh lemongrass are entrapped
in oil glands under parenchyma tissue cell that
restricts the citral from release.
Freeze-dried lemongrass powder showed the highest
of citral concentration (321.41 ± 19.97 ppm) followed
(2) by oven-dried (155.44 ± 16.22 ppm) and vacuum-
(E) (1) dried lemongrass (123.13 ± 17.69 ppm) powder. This
result can be explained that freeze drying method
might preserved the citral compound of lemongrass
powder by minimizing degradation of the compound.
It was in good agreement with Ebadi et al., (2015) who
Fig. 2. Gas Chromatography-Flame Ionization reported that the composition of citral compound on
Detector chromatogram of A) Standard Citral, B) lemon verbena was well –preserved after freeze-
Fresh lemongrass, C) Oven dried, D) Vacuum drying at 64.7 % compared to oven drying (60oC) and
dried and E) Freeze dried of lemongrass powder; vacuum drying (60oC) at 56.7% and 55.5%
Peak identification: (1) neral (cis – Citral) and (2) respectively.
geranial (trans - citral)

Asian J Agric & Biol. 2019;7(1):93-102. 98

Muhamad Asri Hashim al
In addition, freezing caused a minor cellular lemongrass powders (Figure 2). It is possible for
disturbance with inhibiting release of aroma volatile compounds to release from the plant's
compounds (De Ancos et al., 2000). The enzymatic structure to the atmosphere due to the microstructure
reaction is preventable and volatile compounds are changes from drying such as through plant's cell
restricted from release to the surrounding at low expansion (An et al., 2016) as previously observed on
temperature (Palacios, 2014). Furthermore, the effect the cell structure of the freeze-dried parsley (Díaz –
from freezing caused solid phase micro-extraction Maroto et al., 2002) and spearmint (Díaz – Maroto et
become more efficient toward the monoterpene of al., 2003).
citral adsorption as agreed by Díaz-Maroto et al.,
(2002) on extracting sesquiterpenes compounds of Conclusion
spathulenol and β-eudesmol from parsley.
Figure 3 also showed that citral concentration of oven- In conclusion, this study showed that moisture content
dried and vacuum-dried lemongrass powder was and total yield of lemongrass powders were not
insignificant (p>0.05) to each other. Thermal drying significantly (p<0.05) affected by different drying
leads to oxidation, rearrangement and degradation methods. Freeze drying was able to retain the colour
reaction in the presence of oxygen causing a of the lemongrass powder with highest L* value and
decrement of the volatile components (Ding et al., lowest in both a* and b* values. The scanning electron
2012). The decrement of citral compound in this study microscopy images revealed that microstructure of the
had a similar effect on decrement on monoterpenes of thermal-dried of lemongrass powders lead to deform
limonene and 1, 8- cineole under heat-oven drying and collapse. Freeze dried lemongrass powder
under drying temperature at 60oC (Khangholil and obtained the highest concentration of citral compound.
Rezaeinodehi, 2008). This study suggested that freeze dried lemongrass
powder potential to be applied in food and beverages
400 product.
Citral concentration (ppm)

a
Acknowledgement
300
The authors are grateful to Universiti Malaysia
200 Terengganu for facilities and financial support from
b Research Acculturation Collaborative Effort (RACE)
b
b grant (Vote No. 56035) to conduct the research
100 project.

0 Contribution of Authors
Fresh Oven dry Vacuum dry Freeze dry
Lemongrass Powder Hashim MA: Conducted experiment, analysed the data
and drafted the manuscript (master student for this
Fig. 3. Citral concentration (n=3) of lemongrass research project)
powder from different drying methods. Yahya F: Planned the experimental design, read and
Bar with different superscript letters is significantly approved the final draft of manuscript (Leader of this
different (p < 0.05). research project/supervisor)
F: Fresh lemongrass stalk; OD: Oven dried Mustapha WAW: Planned the experimental design,
lemongrass powder, VD: Vacuum dried read and revised the manuscript (co-researcher
lemongrass powder, FD: Freeze dried lemongrass /mentor of this research project)
powder
Disclaimer: None.
The citral concentrations were found to be affected by
Conflict of Interest: None.
the microstructure of lemongrass powders. The
thermally dried powders were exhibited of collapsed Source of Funding: Research Acculturation
fibre with stress-wrinkle structure. Small pores were Collaborative Effort (RACE) grant (Vote No. 56035).
detected during microscopic observation on the

Asian J Agric & Biol. 2019;7(1):93-102. 99

Muhamad Asri Hashim al

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