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Effect of the Temperature on the Spray Drying

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Plant Foods Hum Nutr (2009) 64:6267

DOI 10.1007/s11130-008-0103-y

ORIGINAL PAPER

Effect of the Temperature on the Spray Drying of Roselle

Extracts (Hibiscus sabdariffa L.)
Salvador Gonzalez-Palomares &
Mirna Estarrn-Espinosa &
Juan Florencio Gmez-Leyva & Isaac Andrade-Gonzlez

Published online: 10 December 2008

# Springer Science + Business Media, LLC 2008

Abstract The effect of the drying temperature on the

volatile components and sensory acceptance of the Roselle
(Hibiscus sabdariffa) extract in powder was investigated.
The Roselle extraction was carried out by maceration with
7 L of 30% ethanol (v/v), 560 g of fresh Roselle calyces for
168 h. The Roselle extracts were spray dried at different
temperatures 150, 160, 170, 180, 190, 200 and 210 C,
giving different outlet values about yield and final moisture.
The volatile compounds in Roselle extract and dried
samples were performed using needles of solid phase
microextraction (SPME) and gas chromatography/mass
spectrometry (GC/MS HP-5890). Twenty volatile compounds were identified in the extracts among them
terpenoids, esters, hydrocarbons and aldehydes. Fourteen
volatile compounds were identified in the powder sample,
but only ten were present in the Roselle extract. This
indicates that some compounds were lost and some others
were generated due to a degradation process. An acceptS. Gonzalez-Palomares : J. F. Gmez-Leyva :
I. Andrade-Gonzlez (*)
Graduate and Research Studies Department,
Instituto Tecnolgico de Tlajomulco,
Km. 10 Carr. San Miguel Cuyutln,
CP 45640 Tlajomulco de Ziga, Jal., Mxico
e-mail: isaacag2001@yahoo.com.mx
S. Gonzalez-Palomares
e-mail: chava1142@yahoo.com.mx
J. F. Gmez-Leyva
e-mail: jfgleyva@hotmail.com
M. Estarrn-Espinosa
Centro de Investigacin y Asistencia en Tecnologa
y Diseo del Estado de Jalisco, A.C. Av.,
Normalistas No. 800. Colinas de la Normal,
CP 44270 Guadalajara, Jal., Mxico
e-mail: mestarron@ciatej.net.mx

ability sensory analysis showed that the best powder sample

was the Roselle extract dehydrated using temperature
between 190 C and 200 C (p<0.05). There was not
statistically significant difference in the pH of Roselle
extracts ranging from 3.4 to 3.9. It was concluded that the
spray drying temperature of the Roselle extracts has an
effect on the volatile compounds losses.
Keywords Roselle powder . Sensory analysis . Spray dryer .
Volatile components

Introduction
Roselle calyx (Hibiscus sabdariffa) is the plant part of
greatest interest because the calyx is utilized in the
processing of fruit preserves, jellies and jams for its rich
content in pectin, ascorbic acid and anthocyanin color [1
3]. Today, the Roselle calyces are utilized as a good source
of natural food colorants by their high natural pigment
content [46]. In addition, Hibiscus sabdariffa anthocyanins have been reported to possess antioxidative, antitumor
and anticarcinogenic activity [79]. Nevertheless, Hibiscus
sabdariffa anthocyanins are unstable during the heat treatments, therefore studies on drying process conditions are
requested in order to achieve the best stability of the final
product [10]. The obtaining of Roselle powder through
spray drying is an important alternative method for the use
of the calyces [1113]. The dehydrated products then can
be added easily to other foods to improve their storage,
transportation and shelf-life. This classifies the spray drying
method as the best alternative to obtain colorants and
natural powder flavoring [1416]. Many studies on Roselle
(Hibiscus sabdariffa) powder have been focused on the
factors that are influencing the reconstitution characteristics

Plant Foods Hum Nutr (2009) 64:6267

or the effects of some additives and processes on characteristics of agglomeration and granulation, in addition of
anthocyanin concentrates and the processing conditions,
and physicochemical characteristics of the powder produced [12]. Although the spray drying is a fast process,
changes on the spray drying temperature can affect the
concentration of volatile compounds which would generate
the loss of some sensorial characteristics [1720]. In spite
of the knowledge that the volatile compounds show low
stability at the spray drying temperatures, only scare studies
have been reported on this issue for volatiles in Roselle [6].
To diminish some degradation effects of compounds and
lost of volatile products is very common to use encapsulation agents [21, 22]. For this reason, the extraction of
volatile substances by micro extraction in a solid phase
(SPME), the quantitative and qualitative analysis by gas
chromatography and mass spectrometry (GC-MS) as well
as sensorial assays are useful tools in the evaluation of the
effect of certain process variables about the quality of the
dehydrated products [2326].
The objective of this work was to evaluate the effect of
the spray drying temperatures on the Roselle extracts
(Hibiscus sabdariffa L.), the retention of the volatile
compounds and the sensorial acceptance of the reconstituted spray dried samples.

Materials and Methods

Roselle Extracts Samples
Fresh Roselle calyces (with 79% humidity) were collected
from an experimental field in Michoacan, Mexico during
October and November 2006. The fresh calyces were
washed for quick dipping over water distilled. After the
calyces were crushed manually and deposited in a closed
container with 7 L of 30% methanol (v/v), all under
constant conditions of static maceration. The content was
left in maceration for 168 h with an occasional shaking to
increase the extraction capacity at room temperature. After,
the macerated extracts were filtered through a 150 m
mesh. A Bchi rotavapor was used to concentrate the
samples and to separate all the ethanol at 40 C. The
characteristics of the roselle extracts were 22% of soluble
solids and pH of 3.4. The roselle extracts were kept under
refrigeration at 4 C. An ATAGO refractometer was used to
determine the percentage of soluble solids. An ORION
potentiometer was used to measure the pH.
Spray Drying
A NIRO spray dryer (with the capacity to evaporate 40 kg
of water per hour) with a wheel rotating atomizer was used

63

for the spray drying process in all the experiments. The

outlet temperature was fixed in 80 C and the atomization
was kept at 37,788g. A flexible plastic tube was inserted
inside one container and connected to a variable flow
peristaltic pump. The flexible outlet tube from the pump
was directly connected to the liquid fed inlet of the
atomizer. Seven different spray drying temperatures were
used; 150, 160, 170, 180, 190, 200 and 210 C. The Roselle
powder samples obtained by spray drying were weighed
and packed in their respective amber-coloured glass flasks
of 100 mL. These were stored in containers with silica for
future analysis.
Determination of Moisture in the Spray Dried
Samples of Roselle
In the samples of spray dried Roselle the percentage of
moisture was measured by the method of the vacuum stove
according to the AOAC-934.06 [27]. Six grams of each
sample were placed in an aluminum dish and introduced in
a vacuum stove with a temperature of 40 C until the
weight remained constant.
Reconstitution of Roselle Powder
The reconstituted samples were carried out by placing a
portion of Roselle powder in 300 mL of distilled water. A
magnetic stirrer was used for mixture homogenization. The
standardization of the mixture was carried out in all the
samples until reaching the same concentration of soluble
solids of the liquid extract (22%) [12]. The reconstituted
samples were stored in amber-colored glass flasks and
refrigerated until their analysis.
Volatile Analysis of Roselle Extracts by SPME-GC-MS
The extraction of volatile compounds from the matrix of the
Roselle extracts was carried out by solid-phase microextraction (SPME). Twenty milliliters of Roselle extract
were placed in a 40 mL amber headspace vial. The vial was
fitted with a PTFE-faced silicone septum and put in a
thermostatted bath. A fiber coated with 50/30 mm of
divinylbenzene/carboxen on polydimethylsiloxane (DVB/
Carboxen/PDMS, Supelco, Bellefonte, PA) exposed for
30 min at 60 C in the headspace of the vial was then
immediately inserted into the injection port of the gas
chromatograph for 5 min at 240 C [28]. A HewlettPackard 5890 Series II gas chromatograph with flame
ionization detector (FID) coupled to 5972 MSD quadrupole
mass spectrometer was used. The HP5890 chromatograph
was equipped with HP-1 (50 m0.2 mm ID0.33 m film
thickness) a capillary column. Operating conditions for GC/
MS were: the oven temperature was programmed at 40 C

64

Plant Foods Hum Nutr (2009) 64:6267

for 5 min then ramped at 5 C/min to 240 C, helium with a

flow rate of 0.8 mL/min, injector port and detector temperatures were 220 and 260 C. All the samples were run at
least in triplicates. Volatile compounds were identified by
comparison of their retention indices tentatively only by
mass spectra library Wiley 275L. Quantitation was based in
area percent corresponding to the identified components in
the Total Ion Chromatogram (TIC).
Sensorial Analysis
All the powder samples were reconstituted at 12% of soluble
solids and slightly sweetened with sugar. The control was the
original extract. All the reconstituted samples were evaluated
for sensorial acceptability by pairing a preference test. The
panel participating in the acceptance evaluation included 50
volunteers (50% females 1845 years), who were students
and staff members of the Technological Institute of the West
Mexico, Jalisco Campus. These panelists were randomly
selected based on availability, interest and regular consumption of Roselle drinks.
The reconstituted samples were chilled at 5 C for 24 h
prior to sensory evaluation. Each panelist received the
reconstituted sample in a random order, and a glass of water
for rinsing and crackers for consumption between samples
were supplied. Each panelist was served with 10 mL of
chilled reconstituted samples and control in 30 mL clear
plastic containers, which were randomly coded. In this
paired preference test, panelists were asked to make a
forced choice between the drinks [2, 4, 29]. This test was
used as a measurement of relative preference of one Roselle
drink over another.
Statistical Analysis
An Analysis of Variance (ANOVA) using the Statistical
Analysis System Software (SAS) and Duncan test at
(p>0.05), was performed with the data obtained from GCMS. Also, analysis of significant minimum difference
(DMS) was made, among the Roselle powders to determine
differences based on the pick area of each volatile
component. The peak areas identified by GC-MS were
used as variables. The paired preference data were analyzed
by binomial distribution [23].

Results & Discussion

Spray Drying of Roselle Extracts
The processing conditions for all the spray drying experiments
were kept at the outlet temperature (80 C) and the atomizer
rate (26,000 rpm). In all experiments, Roselle powder showed
a noticeable tendency to stick to internal stainless steel surfaces
of the drying chamber especially at higher inlet temperature
because this temperature increase the feed flow rate [12]. This
is probably due to the nature of the soluble solids. The
adherence of powder to walls of the drying chamber is a
commonly recognized effect in spray drying of solutions
containing sugars and solids easy to agglomerate [30].
The weight, moisture and pH of seven Roselle powder
samples obtained by spray drying at different temperature
are shown in Table 1. It is observed that the pH of the
powder does not change with different temperature treatment;
the name of current Roselle variety and the cited one should be
mentioned [1, 12].
Volatile Compounds Identified in the Roselle Extract
by SPME and GC-MS
In the Roselle extract, 20 volatile compounds were
identified. In general, there were terpene components,
esters, aldehydes and phenolic derivatives. However, only
the terpene compounds were similar to another works [6].
These compounds were limonene, linalool and alphaTerpineol. This has two significant reasons: first, the variety
of the Roselle is different; this indicates that each variety
can have different compositions. The second is that the
isolation method of volatile compounds used in this work
did not require boiling temperatures, only required an
appropriate material of the fiber (DVB/Carboxen/PDMS)
and a temperature of 60 C. This implies that the
degradation problem in the samples of powder Roselle
extracts were not gendered by the SPME analysis method.
Volatile Compounds of the Roselle Powder
The Roselle powder was rehydrated to the same soluble
solid concentration than the liquid extract to determine the
volatile compounds. In these samples 14 volatile com-

Table 1 Weight (grams), moisture percentage and pH of the Roselle powder dried at different temperatures
Treatment
Spray drying temperature (C)

T1
150

T2
160

T3
170

T4
180

T5
190

T6
200

T7
210

Weight (g)
Humidity (%)
pH

73
5.0
3.48

74
4.0
3.48

74
4.0
3.44

78
4.0
3.44

80
3.0
3.44

75
3.0
3.48

74
3.1
3.48

Plant Foods Hum Nutr (2009) 64:6267

65

pounds were identified. Ten of the 14 compounds identified

are the same as the ones identified in the liquid extract,
although there was a decrease in their concentration. Four
different compounds were also generated, derived of the
degradation of sugar and fatty acids that were present in the
liquid Roselle extract [6]. In Table 2 the compounds of
the Roselle powder are shown and the chromatograms are
illustrated in Fig. 1.
The compounds generated by chemical degradation of
the samples during the spray drying were the furfural, cislinalool oxide, furanic linalool oxide Z and E, and the
eugenol. It was observed that the concentration of the
furfural increased because the drying temperature propitiated its formation by degradation of sugars. The cis-linalool
oxide and the furanic linalool oxide Z and E were the product
of the chemical degradation of the fatty acids. The eugenol
is a compound resulting from degradation of the phenolic
compounds as a consequence of the spray drying temperature of the Roselle samples. This also was reported in drying
Roselle calyces [6]. In Fig. 2 is shown the upward behavior
of the furfural, cis-linalool oxide, furanic linalool oxide Z

and E and eugenol compounds due to the obtained the

changes by the spray drying temperature.
Duncans test (p<0.05) determined that exist significant
difference among the seven treatments realized to obtain
Roselle powder at different spray drying temperatures.
The Duncans test was based on the percentage area of the
volatile compounds. Only the compounds the alphaterpinolene, ethyl hexadecanoate, and decanal compounds
were present in all experiments without significant
difference, as shown in Table 2. According to the analysis
of the least significant difference (LSD) carried out among
the Roselle powder samples, the Roselle extract dehydrated
at 190 C presented the biggest concentration of volatile
compounds and the least concentrations of degraded
compounds that the other samples obtained from different
spray drying temperatures, as shown in Table 2. This result
proved the hypothesis that the drying temperature had an
effect on the retention of volatiles compounds. In addition,
it is important to acknowledge that significant differences
exist among the compounds identified in the liquid extract
as the compounds identified in the Roselle powder. This

Table 2 Volatiles identified in the Roselle powder

Spray drying temperature (C)
Area (%)
T150
150 C
Volatile compounds retained in the powder
Terpenoids
p-Cymene
0.10 ab
Limonene
1.70 ab
Alpha-Terpinolene
0.10 a
Linalool
0.10 b
Esters
Ethyl hexadecanoate
1.70 a
Ethyl linoleate
0.53 b
Ethyl linoleolate
0.10 c
Aldehydes
Benzaldehyde
0.07 c
Decanal
0.18 a
Divers
4-Ethylguaiacol
0.06 b
Volatile compounds generated by chemical degradation
Sugar derivatives
Furfural
0.30 d
Phenolic derivatives
Eugenol
0.09 c
Fatty acid derivatives
cis-Linalool oxide
0.76 b
Furanic linalool oxide Z and E
0.20 c

T160
160 C

T170
170 C

T180
180 C

T190
190 C

T200
200 C

T210
210 C

0.14
1.60
0.09
0.09

0.12
1.80
0.04
0.05

0.13
1.50
0.06
0.06

0.20
4.00
0.07
0.33

0.12
1.00
0.10
0.25

0.07
0.05
0.08
0.10

ab
ab
a
b

ab
ab
a
b

ab
ab
a
b

a
a
a
a

ab
b
a
ab

b
b
a
b

1.70 a
0.50 b
0.13 c

1.72 a
0.47 b
0.13 c

1.68 a
0.71 ab
0.19 b

1.69 a
0.87 a
0.28 a

1.68 a
0.83 a
0.11 c

1.67 a
0.45 b
0.10 c

0.09 c
0.16 a

0.35 b
0.17 a

0.31 b
0.18 a

0.55 a
0.18 a

0.40 ab
0.16 a

0.05 c
0.16 a

0.06 b

0.07 b

0.07 b

0.13 a

0.06 b

0.02 c

2.51 c

2.69 c

3.80 b

4.00 ab

4.28 a

4.44 a

0.10 c

0.10 c

0.15 b

0.20 b

0.35 a

0.30 a

0.87 b
0.29 b

0.85 b
0.35 b

1.00 ab
0.40 b

1.07 ab
0.51 ab

1.55 a
0.69 a

1.40 a
0.50 ab

Different letters mean statistically significant difference using Duncan (p<0.05). Multiple range tests with base in their retention

66

Plant Foods Hum Nutr (2009) 64:6267

Fig. 1 Chromatogram of
volatile constituents in Roselle
powder dried at 190 C. The
time is in minutes

indicates that it is difficult to obtain a powder exactly

similar to the liquid extract of Roselle.
Sensorial Analysis
According to the sensorial analysis, more than 76% of the
panelists showed that preference for the sample T190 than
corresponded to 190 C drying outlet temperature, although
the liquid extract has 92% of preference in the same
conditions (T0). In comparison to the other treatments
(different temperatures), this had the lowest percentage of
5

preference: T150=16%, T160=40%, T170=52%, T180=

52%, T200=12%, and T210=12%. Figure 3 shows the
percentage over the flavor preference among all the samples
analyzed, where the highest acceptability was for the liquid
extract followed by the T190 sample with statistically
significant differences (p<0.05).
Therefore, it is clear than there is significant difference
on acceptance among the Roselle powders and the original
liquid extract according to the preference tests. The major
components detected by chromatographic analysis played
an important role.

Conclusions

4.5

The inlet air temperature of 190 C used in the spray the

drying of Roselle extract resulted in the best powder in
terms of composition regarding the other treatments, since
it contained the highest concentration of ten volatile com-

Area (%)

3.5
3
2.5
2

100

1.5

90

0.5
0
150

160

170

180

190

200

210

Spray Drying Inlet Temperature (C)

Furfural

Cis-linalool oxide

Furanic linalool oxide Z

and E

Eugenol

Fig. 2 Effect of spray drying temperature on the concentration of

degradation compounds present in Roselle powder

Acceptance (%)

80

70
60
50
40
30
20
10
0
T0

T150

T160

T170

T180

T190

T200

T210

Treatments at different temperatures (C)

Fig. 3 Results of the paired preference tests of the Roselle

reconstituted powder. T0 is Roselle liquid original extract

Plant Foods Hum Nutr (2009) 64:6267

pounds also showed in the original liquid extract, and the

peak area of the degraded compounds is smaller than other
samples treated at higher temperature. This result was
rehearsed for panelists in the preference test, choosing the
T190 sample as the best after the original extract, with an
acceptability of 76%. This work suggests that the inlet air
temperature of spray drying has a significant effect on the
volatile compounds concentration of the Roselle liquid
extract and therefore in its acceptance.
Acknowledgement We thank their support in this investigation to
the ITA-JAL, DGETA, CoSNET and CIATEJ.

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