Journal of Food Engineering 93 (2009) 421426

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Journal of Food Engineering

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Extraction of vanillin from vanilla pods: A comparison study of conventional

soxhlet and ultrasound assisted extraction
Dnyaneshwar Jadhav, Rekha B.N., Parag R. Gogate, Virendra K. Rathod *
Chemical Engineering Department, Institute of Chemical Technology, Matunga, Mumbai-40019, India

a r t i c l e i n f o a b s t r a c t

Article history: This study deals with extraction of vanillin from cured vanilla pods using conventional soxhlet extraction
Received 13 June 2008 and ultrasound assisted extraction. Effect of various extraction parameters such as type of the solvent (6
Received in revised form 5 February 2009 different solvents viz. ethanol, methanol, acetonitrile, acetone, chloroform and hexane), quantity of beans
Accepted 8 February 2009
(13 g), operating temperature (in the range 90100 C) for soxhlet extraction and pre-leaching time (in
Available online 20 February 2009
the range of 3090 min) for ultrasound assisted extraction, on the extent of extracted vanillin has been
investigated in this work. It has been conclusively established that the use of polar solvents resulted in
Keywords:
maximum extent of extraction for both the types of extraction operations. For soxhlet extraction, an
Extraction
Ultrasonic irradiation
increase in operating temperature from 90 C to 100 C was found to increase extent of extraction by
Vanillin 30% whereas for ultrasound assisted extraction, pre-leaching stage for 30 min duration was found to
Vanilla pods be benecial in enhancing the extent of extraction by about 20%. The use of ultrasonic irradiation resulted
Process intensication in intensication of the extraction operation of vanillin signicantly as conrmed from the results that in
soxhlet extraction, an operating temperature of 95 C and solvent to solute proportion of 66.67 ml/g
(most commonly used conditions) resulted in release of around 180 ppm in 8 h whereas ultrasonic
assisted extraction required only 1 h for release of around 140 ppm vanillin concentration at similar pro-
portions of solvent to solute and under ambient operating temperature.
2009 Elsevier Ltd. All rights reserved.

1. Introduction sumption of natural vanillin and the growing preference by con-

Vanillin is one of the most widely used avor resources in con-
fectionery, food products, beverages, ice-cream industries as avor,
perfumes and in pharmaceutical preparations (Sinha et al., 2008).
In addition, vanillin is also active against Germ-positive and
Germ-negative food spoilage bacteria, yeasts and moulds in fruit
purees and laboratory growth media and has considerable poten-
tial for use as a food preservative. Vanillin is generally produced
from ground black vanilla bean pods. Vanillin (4-hydroxy-3-
methoxybenzaldehyde) principally is one of the worlds popular
avor extracts obtained primarily from Vanilla planifolia, specie
of tropical climbing orchid native to Mexico, but currently culti-
vated in many countries such as Madagascar, Indonesia, Tahiti
and Tonga (Esposito et al., 1997). Vanillin can also be obtained
through various methods like chemical synthesis, biotransforma-
tion, from degradation of waste sulte liquors apart from extrac-
tion of natural vanilla pods which contain about 23% w/w
vanillin (Esposito et al., 1997; Rao and Ravishankar, 2000; Bedou-
kian, 1986; Zhao et al., 2005). Moreover, vanillin has also been re-
ported in traces in many plants including tobacco and fruits and
fruit products such as orange, grapefruit and tangerine. High con-
* Corresponding author. Tel.: +91 22 24145616; fax: +91 22 24145614.
E-mail address: vkr@udct.org (V.K. Rathod).
sumers for using natural avors due to food safety concerns have
highlighted the need for developing environmentally benign
extraction methods for obtaining such ingredients from natural
sources.
Extraction of biologically active components from plant is one
of the more sustainable approaches that may be employed. Con-
ventionally, a range of methods including solvent extraction,
supercritical uid extraction etc., are employed to recover the nat-
ural products. The selection of the method to isolate active compo-
nents with best yield and highest purity from natural sources is
mainly dependent on the nature of compounds and raw material
to be processed. These extraction techniques are often limited by
the mass transfer resistances due to involvement of more than
one phase in the system. Cavitation generated using ultrasound
is known to produce physical effects such as liquid circulation cur-
rent and turbulence which can aid in elimination of decreasing
mass transfer rates. Indeed, the use of ultrasound has been re-
ported to increase the yield and rate of mass transfer in several so-
lidliquid extraction processes (Thompson and Sutherlands, 1955;
Romdhane and Gourdon, 2002; Vinatoru, 2001). The mechanism of
intensication of extraction process has been attributed to cavita-
tion phenomena resulting in intense turbulence and liquid circula-
tion currents in the system. Vinatoru (2001) has reviewed various
applications of ultrasound in intensication of extraction of bioac-

0260-8774/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2009.02.007
422 D. Jadhav et al. / Journal of Food Engineering 93 (2009) 421426
tive materials from herbs. Some of the other recent applications in-
clude extraction of hesperidin from Penggan (Citrus reticulata)
peel (Ma et al., 2008), extraction of rutin and quercetin from Euon-
ymus alatus (Thunb.) Sieb (Yang and Zhang, 2008), extraction of
phenolic compounds from coconut (Cocos nucifera) shell powder
(Rodrigues et al. 2008) and extraction of oil from tobacco (Nicoti-
ana tabacum L.) seeds (Stanisavljevic et al. 2007). To the best of
our knowledge, none of the investigations involve the use of inten-
sication of extraction of vanillin from vanilla beans or pods. This
work reports the use of ultrasound assisted extraction for extrac-
tion of vanillin and also its comparison with the conventional sol-
vent extraction process. Optimization of different operating
parameters has also been investigated.
2. Materials and methods
2.1. Materials
The cured vanilla beans were supplied by Vanilco India Ltd. In-
dia. Ethanol, methanol, acetonitrile, acetone, chloroform and hex-
ane used in the experimental work were all of analytical regent
grade chemicals (S-D ne chemicals limited, Mumbai). p-hydroxy-
benzoicacid, p-hydroxybenzaldehyde, vanillic acid, and vanillin
used for analysis were laboratory reagent (LR) grade chemicals
(S-D ne chemicals limited, Mumbai). Methanol and acetic acid
used for HPLC analysis are liquid chromatography (LC) grade
chemicals (E. Merck, Mumbai).
2.2. Conventional extraction (soxhlet extraction)
Fig. 1 gives a schematic representation of the experimental set-
up used for soxhlet extraction. The powdered cured vanilla beans
(2 g) were packed in lter paper and placed in thimble holder.
The arrangement is such that vapors of the solvent are generated
from the reservoir, pass through the thimble and get condensed
in the condenser. The condensed fresh solvent comes in contact
with the cured vanilla beans in the thimble where extraction oc-
curs. When the liquid reaches the overow level in the thimble,
the liquid moves through the siphon back into the reservoir, carry-
Fig. 1. Schematic representation of experimental setup for soxhlet extraction.
ing extracted solutes into the bulk liquid. In solvent ask, solute is
separated from the solvent using distillation. Solute is left in the
ask and solvent vapors pass back into the solid bed material via
the condenser for next cycle of extraction.
Effect of type of solvent (quantity as 200 ml) was investigated in
the case of soxhlet extraction by performing experiments at 95 C
(temperature of bath surrounding the solvent reservoir) using six
different solvents viz. hexane, chloroform, acetonitrile, acetone,
methanol and ethanol (in increasing order of polarity; hexane is
a non-polar solvent whereas polarity increases from chloroform till
ethanol). It should also be noted that though in the current study
the selection of solvents is based on the differences in polarity
and yielding maximum cavitational intensity (due to lower boiling
point and viscosity) for benecial effects, its toxicity needs to be
carefully considered especially where nal application is in food
industries (proper separation techniques need to be established
for removal of even traces of solvents from nal product). Effect
of quantity of beans (13 g) and temperature of the bath (90
100 C) on the extent of extraction was also investigated.
2.3. Ultrasound assisted extraction (UAE)
The experimental setup used for ultrasound assisted extraction
has been depicted schematically in Fig. 2. Ultrasonic horn (Sonics
vibra cell model with 1 cm diameter) operating at 240 W power
dissipation (xed) and frequency of 22.4 kHz was used for the
extraction. Ultrasonic horn was operated in pulsed mode (5 s on
followed by 5 s off) and operated at maximum supplied power.
The actual energy dissipation into the system as measured calori-
metrically (Gogate et al., 2001) was 34 W. Due to pulsed operation
there was not much heating of the solvent. Use of water bath
around the extraction ask also ensured that temperature of the
solvent reservoir did not increase drastically.
During a typical extraction operation, 1 g of cured vanilla bean
was powdered in an electric grinder and mixed with 100 ml of sol-
vent (to keep ratio of solute to solvent similar as to soxhlet extrac-
tion, 1 g of cured vanilla beans were used in 100 ml of solvent).
Ultrasonic irradiations were used for a period of 1 h. Samples were
taken at regular intervals (10 min) for analysis. The concentrated
Fig. 2. Schematic representation of experimental Setup for ultrasound assisted
extraction (UAE).
 D. Jadhav et al. / Journal of Food Engineering 93 (2009) 421426 423

extracts were re-dissolved in 95% ethanol to get sample solution 160

for HPLC analysis. chloroform ethanol
Effect of type of solvent and quantity of vanilla beans were also methanol acetone
140
investigated in the UAE similar parameter ranges as in the conven- acetonitrile hexane
tional extraction. Additional studies were also performed in the

Vanillin concentration (ppm)

case of UAE based on a pre-leaching stage. The aim of pre-leaching 120
was to enhance the permeability of the cell wall to beneciate in-
creased recovery in the actual ultrasound assisted extraction, 100
which follows the pre-leaching stage.
80
2.4. Analysis of vanilla extract

Quantication of vanillin in vanilla extract at low pH is difcult, 60

because vanillin glycosides in vanilla extract may be hydrolysed to
vanillin during HPLC analysis resulting in higher percentage of van-
illin in the overall analysis (Waliszewski et al., 2007). Samples
withdrawn from soxhlet extraction (conventional) and ultrasound
extraction was diluted to second dilution in 95% ethanol and sub-
jected for the analysis. All the solvents used for analysis were HPLC
grade. For sample and solvent ltration, 0.45 lm membrane lters
(Millipore, Germany) were used, and solvents were degassed prior
to use.
Four avor and fragrance constituents of natural vanilla extract
are identied by HPLC (high performance liquid chromatography)
to be vanillin, p-hydroxybenzoic acid, p-hydroxybenzaldehyde
and vanillic acid. The HPLC unit was from Knauer with Knauer
C18 (reverse Phase) vertex column of 250  4 mm cross-section
packed with Eurosphere 100-5 C18. In a typical HPLC run, metha-
nol/acidied water (water was acidied by adding 4 ml of acetic
acid/800 ml) was used as a mobile phase at a ow rate of
0.80 ml/min. The total injection volume for analysis was 20 ll
and UV detector at 270 nm wavelength was used.
2.5. Statistical analysis of the experimental data
Reproducibility of the obtained experimental data is very
important in investigation of effects of the operating parameters
with an aim of optimization of the extraction efciency. In this
study, all the experiments were carried out in triplicates to
estimate the repeatability of the obtained data. The data were
analyzed by descriptive statistics tool provided by Excel, MS Ofce
2003. The graphs were plotted using mean values obtained
from the data. The standard deviation of the replicate values is
shown as error bars in the values depicted on Y axis. All the exper-
imental errors were found to be within 2% of the mean reported
value.
The obtained results were also analyzed using statistical analy-
sis methodologies for establishing the controlling operating
40
20
0
0 1 2 3 4 5 6 7
Time ( hr )
Fig. 3. Effect of different solvents on the extent of vanillin extraction in soxhlet
extraction at an operating temperature of 95 C and using 2 g of vanilla beans in
200 ml of solvent.
and least in the case of non-polar solvent such as hexane. The ex-
tent of extraction of vanillin from cured vanilla beans was the max-
imum in ethanol and hence ethanol was proposed as an optimum
solvent for maximum yield of vanillin.
Vanilla aroma can also be obtained from other volatile constit-
uents present in vanilla pods such as vanillic acid, p-hydroxybenz-
aldehyde and p-hydroxybenzoic acid (Ranadive, 1992). It was
thought worthwhile to investigate the extent of extraction of these
constituents. The results obtained using different solvents have
been shown in Fig. 4. Extraction of vanillic acid and p-hydroxyben-
zoic acid was observed to be maximum in methanol due to high
solubility of vanillic acid and p-hydroxybenzoic acid in methanol.
However extraction of p-hydroxybenzaldehyde was higher in eth-
anol due to its high solubility as compared to other solvents used
in the study. It should also be noted that Vanillic acid, p-hydroxy-
16
PHB acid
14
PHB aldehyde
Concentration (ppm)

12 VA
parameters. The analysis was done using Sigma Stat version 3.5
software supplied by Cranes Software International Limited. 10

8
3. Results and discussion
6
3.1. Conventional extraction (soxhlet extraction) 4

3.1.1. Effect of different solvents on vanillin extraction 2

Solubility of different natural products vary with different sol-
vents i.e. polar solute is soluble in polar solvents like methanol, 0
acetontrile
methanol

chloroform

acetone
ethanol

hexane

ethanol, dimethyl formamide (DMF), etc; whereas non-polar sol-

utes dissolve in non-polar solvents like hexane, benzene, cyclohex-
ane, toluene, etc. The solubility of the natural products also usually
increases with an increase in the polarity levels. Effect of different
solvents on the extent of extraction has been investigated and the
Fig. 4. Effect of different solvents on extent of vanillic acid, p-hydroxybenzoic acid,
results have been shown in Fig. 3. It was observed that extraction p-hydroxybenzaldehyde in soxhlet extraction at an operating temperature of 95 C
of vanillin was higher in polar solvents such as ethanol, methanol and using 2 g of vanilla beans in 200 ml of solvent.
424
benzaldehyde and p-hydroxybenzoic acid are present in much
lower quantity as compared to vanillin as indicated by nal
concentrations.
3.1.2. Effect of quantity of beans on vanillin extraction
Effect of quantity of vanilla beans (in the range 13 g) on the ex-
tent of vanillin extraction was investigated at a constant quantity
of ethanol (200 ml) solvent. The obtained results have been shown
in Fig. 5. It can be seen from the gure that the extent of vanillin
extracted per unit vanilla beans (present initially) depends on
the relative proportions of the vanilla beans and solvent. For the
case of initial quantity of vanilla beans as 1 g (maximum relative
proportion of solvent), the rate of extraction almost follows a linear
path with time of operation, whereas for initial quantity as 3 g
(minimum relative proportion of the solvent), the rate of extraction
decreased with extended extraction time. Comparing the nal
amounts after 8 h of extraction, the extent of vanillin extraction
per unit initially present vanilla beans is minimum for solvent pro-
portion as 66.67 ml/g, it increases by about 50% when the solvent
proportion is increased to 100 ml/g and then only marginally in-
creases for solvent proportion as 200 ml/g. Based on these results
an optimum operation proportion of solvent to solute was selected
as 100 ml of solvent to 1 g of vanilla beans.
3.1.3. Effect of temperature on vanillin extraction
In the case of conventional soxhlet extraction the rate of recycle
of the condensed solvent should also play a role in deciding the ex-
tent of extraction as it is essentially mass transfer controlled oper-
ation. The rate of recycle can be indirectly controlled by modifying
the rate of vapor generation and ensuring sufcient cooling capac-
ity for complete condensation. Considering this background, the ef-
fect of temperature of oil bath in the range of 90100 C has been
investigated in the current work and the obtained results have
been depicted in Fig. 6. It can be seen from the gure that the ex-
tent of extraction of vanillin increased with an increase of oil bath
temperature. An increase in the temperature of bath is likely to in-
crease the rate of recirculation of the solvent through the extrac-
tion zone and hence the extent of extraction increases.
100
1 g Vanilla beans
Vanillin concentration per unit vanilla beans
90
2 g Vanilla beans
80 3 g Vanilla beans
70
60
50
40
30
20
10
0 with respect to contact time and the extent of recovery beyond
0 2 4 6
Time (hr)
Fig. 5. Effect of quantity of vanilla beans on vanillin extraction in Soxhlet extraction
at an operating temperature of 95 C and using constant quantity of ethanol as
200 ml.
D. Jadhav et al. / Journal of Food Engineering 93 (2009) 421426
200
90C 95C 100C
180
160
Vanillin concentration (ppm)
140
120
100
80
60
40
20
0
0 2 4 6 8 10
Time (h)
Fig. 6. Effect of bath temperature on vanillin extraction using Soxhlet extraction
using 1 g of vanilla beans in 100 ml of ethanol.
3.1.4. Statistical analysis of the obtained results
Statistical analysis of the obtained variations for different oper-
ating parameters such as type of solvent, operating temperature
and relative proportion of the solvent to the quantity of vanilla
beans in the case of soxhlet extraction was done in order to estab-
lish the contributing independent variables to the dependent var-
iable as the amount of vanillin extracted. As the effect of type of
solvent was not quantiable in terms of a single parameter, effect
of solvent was analyzed on the basis of the Rank-Percentile test of
Excel (MS Ofce 2003). It was observed that the order of effect of
solvent on the extraction efciency is as follows: ethanol > metha-
nol > acetone > acetonitrile > chloroform > hexane. Among the
other two quantiable variables i.e. operating temperature and rel-
ative proportion of solvent to solute, both the parameters contrib-
uted to the overall extraction process (value of P was found to be
less than 0.05). The obtained data also passed the normality test
and the constant-variance test.
3.2. Ultrasound assisted extraction (UAE)
3.2.1. Effect of different solvents on vanillin extraction
In the case of ultrasound assisted extraction, effect of type of
solvent was investigated for different solvents similar to soxhlet
extraction and the obtained results have been shown in Fig. 7. It
can be seen from the gure that the extraction of vanillin increased
with an increase in the polarity of the solvent similar to that ob-
served for the conventional extraction process. Similar observa-
tions were also made for other constituents viz. Vanillic acid, p-
hydroxybenzaldehyde and p-hydroxybenzoic acid. Statistical anal-
ysis also conrmed the order of the efcacies of different solvents
as explained in the case of conventional extraction process. An
interesting feature can also be observed from the depicted trends
in Fig. 7. The recovery of vanillin seem to reach a saturation level
8 10
1 h of contact time using ultrasound was only marginal. This indi-
cates that even though ultrasound is intensifying the process as
compared to the conventional soxhlet extraction it has a limitation
in terms of maximum possible recovery from the given amount of
vanilla beans. With this background in mind pre-leaching studies
 D. Jadhav et al. / Journal of Food Engineering 93 (2009) 421426
120
100
Vanillin concentration (ppm)
80
60
40
Chloroform
20
Acetone
Ethanol
0 water structuring by the addition of small amounts of alcohol de-
0 10 20 30 40
Time (minutes)
Fig. 7. Effect of different solvents on vanillin extraction using Ultrasonic assisted
extraction using 1 g of vanilla beans in 100 ml of solvent.
were performed for the ultrasound assisted extraction operation as
the main mechanism of release of vanillin is by disruption of cell
walls.
The dependence of the progress of extraction process on the rel-
ative proportions of the solvent to solute was also investigated by
changing the quantity of vanilla beans at a constant quantity of the
solvent. The obtained trends were again similar to the conven-
tional soxhlet extraction operation and maximum extent of extrac-
tion per unit vanilla beans was observed when maximum
proportion of solvent was used. Quantitatively speaking, after 1 h
of extraction, the extent of vanillin extracted per unit initially pres-
ent vanilla beans is minimum for solvent proportion as 66.67 ml/g,
it increases by about 40% when the solvent proportion is increased
to 100 ml/g and by a further 25% for solvent proportion as 200 ml/
g. It can be seen that when compared with the conventional pro-
cess, the extent of increase in the extraction of vanillin in ethanol
at a ratio of 200 ml/g was higher possibly due to cavitational ef-
fects. In the absence of ultrasound, liberation of the bound vanillin
and their diffusion also occurs, but at much slower rate. Thus, the
action of ultrasonic energy would be to accelerate this rate control-
ling diffusional process and also possibly by enhancing the perme-
ability of the cell walls to facilitate the release of vanillin.
3.2.2. Effect of pre-leaching time on the extraction of vanillin
The pre-leaching procedure usually consists of the soaking and
swelling of the beans in a suitable solvent or mixture of solvents in
the absence of ultrasound and is followed by the extraction proce-
dure in the presence of ultrasound. The aim of pre-leaching stage is
to enhance the permeability of the cell wall to beneciate the in-
crease in release of vanillin in the actual ultrasound assisted
extraction, which follows the pre-leaching stage. The pre-leaching
stage is also expected to enhance the maximum quantum of vanil-
lin extracted.
To determine the effect of pre-leaching time before ultrasound
assisted extraction, experiments were conducted where powdered
cured vanilla beans were pre-leached, in same solvent as used for
ultrasonic extraction, for various time intervals (3090 min) in the
absence of ultrasonic irradiations. After the pre-leaching stage,
ultrasound assisted extraction operation was performed for a per-
iod of 1 h. It has been observed that an pre-leaching time of 30 min
425
enhances the quantity of vanillin extracted after 1 h of ultrasound
assisted extraction by about 20% but further increase in the pre-
leaching time (60 and 90 min) results only in marginal benecial
effects. Thus, it can be said that 30 min duration is sufcient to
achieve possible soaking and swelling of the cells and increase
the permeability of cell walls.
3.2.3. Effect of ethanol concentration on the extraction of vanillin
The structure of vanillin clusters is preserved in aqueous solu-
tions containing low percentages of alcohol or other organic sol-
vents, apparently due to the fact that the hydrophobicity of
organic solvents enhances aromatic stacking (Kappatos et al.,
1996). However, when vanillin is exposed to mostly an aqueous
microenvironment, there might be a diminution in pp stacking
interactions. Moreover, water molecules enveloping vanillin crys-
Methanol tals may form hydrogen bonds that link neighboring vanillin mol-
ecules in a cluster. Hence, an aqueous environment might enhance
Acetonitrile
the solubility of vanillin and, in consequence, break up the multi-
molecular structure of vanillin aggregates. Also, reinforcement of
50 60 70
creases the solubility of vanillin, whereas disruption of water
structure by higher alcohol concentrations greatly enhances sol-
ventsolute interfacing and increased solubility of vanillin (Frenkel
and Havkin-Frenkel, 2006). Thus it appears that an optimum ratio
of alcohol to water might results in maximum amount of vanillin
release. With this background, effect of mixture of waterethanol
on the extent of extraction has been investigated and it was indeed
observed that the extraction of vanillin from cured vanilla beans
was greatly inuenced by the ethanol concentration in water.
When the ethanol volume percentage in the solvent was lower
than 50% (v/v), the extraction increased with the increase of etha-
nol concentration (from about 85 ppm at 20% ethanol to about
120 ppm of vanillin extraction at 50% ethanol). However beyond
this concentration, any further increase was found to be detrimen-
tal for the extraction process (the extent of vanillin extraction de-
creased gradually to about 105 ppm for 100% ethanol). Thus, a
1:1 v/v ethanol/water solution resulted in maximum extraction
of vanillin from cured vanilla beans. This can be attributed to high-
er polarity of solvents containing water facilitated the solubiliza-
tion of vanillin. It can also be conclusively established here that
use of ultrasound also reduces the requirement of the ethanol for
similar levels of extraction of vanillin. Quantitatively speaking
use of pure ethanol in conventional process required about 4 h
for release of 120 ppm concentration of vanillin whereas in the
presence of ultrasound, 1:1 v/v ethanol/water solution (with total
amount of solvent being used remaining the same) resulted in sim-
ilar levels of vanillin after only 30 min of treatment time.
3.3. Comparison of UAE and conventional extraction
Ultrasonic energy denitely has utility in the extraction of van-
illin from cured beans, as it results in a substantial enhancement of
extraction efciency by increasing the diffusion rates by virtue of
eliminating mass transfer resistances. Generally, in soxhlet extrac-
tion the residue was repeatedly exposed to the solvent. During
ultrasonic extraction, this physical separation is further enhanced
by the localized stirring occurring as a consequence of cavitation.
The combination of this stirring effect and the repeated washing
of the vanillin with solvent were far superior to the simple washing
procedure in soxhlet extraction. In all the cases investigated in this
work, the rate of extraction was more rapid with ultrasound than
with soxhlet extraction. Fig. 8 shows the maximum extent of van-
illin recovered using ultrasound assisted and soxhlet extraction
techniques. It can be seen that conventional extraction required
8 h for release of around 180 ppm vanillin concentration at operat-
ing temperature of 95 C and solvent to solute proportion of
426 D. Jadhav et al. / Journal of Food Engineering 93 (2009) 421426
200
180 Soxhlet Extraction Ultrasound
160
Vanillin Concentration (ppm)
140
120
100
80
60
40
20
0 F., 1997. Kirk-Othmer Encyclopedia of Chemical Technology, fourth ed. John
66.67 100 200
Relative proportion of solvent to solute
Fig. 8. Comparison of Ultrasound assisted extraction (time = 1 h) and conventional
extraction methods (time = 8 h).
66.67 ml/g whereas ultrasonic assisted extraction required only
1 h for release of around 140 ppm vanillin concentration at similar
proportions of solvent to solute and under ambient operating tem-
perature. Similar increases using ultrasound has been reported in
the literature. Hromdkov et al. (2008) have reported that for sim-
ilar yields of water-soluble polysaccharides from both extraction
steps and total isolated polysaccharides, ultrasonic irradiation re-
quired 2% NaOH and 5 min of treatment time whereas classical
process required about 80 min of time with 5% NaOH. Fu et al.
(2006) have also reported that ultrasound assisted extraction of
xyloglucan was about three times faster than the traditional
extraction method.
4. Conclusions
This study has enabled us to conrm the role of ultrasound in
enhancing the rates of extraction by a comparison study with the
conventional soxhlet extraction. In both the modes of extraction,
the yield of vanillin in vanilla extract was higher for polar solvents
such as ethanol and for higher proportion of solvent to solute. In
the case of conventional soxhlet extraction use of higher operating
temperatures in the oil bath were found to give enhanced recovery
of vanillin by virtue of higher rates of recycle for the solvent. Short
period of pre-leaching was found to be effective enhancing the ex-
tent of release of vanillin in the UAE by way of enhancing the per-
meability of the cell wall. Compared with the conventional
extraction method (soxhlet), the UAE provided high extraction of
vanillin in much shorter time periods for all the solvents investi-
gated in the current work. It can be suggested that ultrasonic treat-
ment on a commercial scale could be utilized protably and simply
by applying ultrasound to the pre-leached mixture for short time
period.
Acknowledgements
Authors would like to acknowledge the support of Prof. B.M.
Bhanage for valuable suggestions in this work. One of the authors,
Dnyaneshwar Jadhav would like to acknowledge the funding of
UGC.
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