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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.
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- ing extracted solutes into the bulk liquid. In solvent ask, solute is
clude extraction of hesperidin from Penggan (Citrus reticulata) separated from the solvent using distillation. Solute is left in the
peel (Ma et al., 2008), extraction of rutin and quercetin from Euon- ask and solvent vapors pass back into the solid bed material via
ymus alatus (Thunb.) Sieb (Yang and Zhang, 2008), extraction of the condenser for next cycle of extraction.
phenolic compounds from coconut (Cocos nucifera) shell powder Effect of type of solvent (quantity as 200 ml) was investigated in
(Rodrigues et al. 2008) and extraction of oil from tobacco (Nicoti- the case of soxhlet extraction by performing experiments at 95 C
ana tabacum L.) seeds (Stanisavljevic et al. 2007). To the best of (temperature of bath surrounding the solvent reservoir) using six
our knowledge, none of the investigations involve the use of inten- different solvents viz. hexane, chloroform, acetonitrile, acetone,
sication of extraction of vanillin from vanilla beans or pods. This methanol and ethanol (in increasing order of polarity; hexane is
work reports the use of ultrasound assisted extraction for extrac- a non-polar solvent whereas polarity increases from chloroform till
tion of vanillin and also its comparison with the conventional sol- ethanol). It should also be noted that though in the current study
vent extraction process. Optimization of different operating the selection of solvents is based on the differences in polarity
parameters has also been investigated. and yielding maximum cavitational intensity (due to lower boiling
point and viscosity) for benecial effects, its toxicity needs to be
2. Materials and methods carefully considered especially where nal application is in food
industries (proper separation techniques need to be established
2.1. Materials for removal of even traces of solvents from nal product). Effect
of quantity of beans (13 g) and temperature of the bath (90
The cured vanilla beans were supplied by Vanilco India Ltd. In- 100 C) on the extent of extraction was also investigated.
dia. Ethanol, methanol, acetonitrile, acetone, chloroform and hex-
ane used in the experimental work were all of analytical regent 2.3. Ultrasound assisted extraction (UAE)
grade chemicals (S-D ne chemicals limited, Mumbai). p-hydroxy-
benzoicacid, p-hydroxybenzaldehyde, vanillic acid, and vanillin The experimental setup used for ultrasound assisted extraction
used for analysis were laboratory reagent (LR) grade chemicals has been depicted schematically in Fig. 2. Ultrasonic horn (Sonics
(S-D ne chemicals limited, Mumbai). Methanol and acetic acid vibra cell model with 1 cm diameter) operating at 240 W power
used for HPLC analysis are liquid chromatography (LC) grade dissipation (xed) and frequency of 22.4 kHz was used for the
chemicals (E. Merck, Mumbai). extraction. Ultrasonic horn was operated in pulsed mode (5 s on
followed by 5 s off) and operated at maximum supplied power.
2.2. Conventional extraction (soxhlet extraction) The actual energy dissipation into the system as measured calori-
metrically (Gogate et al., 2001) was 34 W. Due to pulsed operation
Fig. 1 gives a schematic representation of the experimental set- there was not much heating of the solvent. Use of water bath
up used for soxhlet extraction. The powdered cured vanilla beans around the extraction ask also ensured that temperature of the
(2 g) were packed in lter paper and placed in thimble holder. solvent reservoir did not increase drastically.
The arrangement is such that vapors of the solvent are generated During a typical extraction operation, 1 g of cured vanilla bean
from the reservoir, pass through the thimble and get condensed was powdered in an electric grinder and mixed with 100 ml of sol-
in the condenser. The condensed fresh solvent comes in contact vent (to keep ratio of solute to solvent similar as to soxhlet extrac-
with the cured vanilla beans in the thimble where extraction oc- tion, 1 g of cured vanilla beans were used in 100 ml of solvent).
curs. When the liquid reaches the overow level in the thimble, Ultrasonic irradiations were used for a period of 1 h. Samples were
the liquid moves through the siphon back into the reservoir, carry- taken at regular intervals (10 min) for analysis. The concentrated
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
chloroform
acetone
ethanol
hexane
200 vanillin in much shorter time periods for all the solvents investi-
gated in the current work. It can be suggested that ultrasonic treat-
180 Soxhlet Extraction Ultrasound ment on a commercial scale could be utilized protably and simply
by applying ultrasound to the pre-leached mixture for short time
160 period.
Vanillin Concentration (ppm)
140
Acknowledgements
120
40 References
Bedoukian, P.Z., 1986. Perfumery and Flavorings Synthesis, third ed. Allured
20
Publishing, Wheaton, USA.
Esposito, L.J., Formanek, K., Kientz, G., Mauger, F., Maureaux, V., Robert, G., Truchet,
0 F., 1997. Kirk-Othmer Encyclopedia of Chemical Technology, fourth ed. John
66.67 100 200 Wiley Sons, New York. pp. 812825.
Relative proportion of solvent to solute Frenkel, C., Havkin-Frenkel, D., 2006. The physics and chemistry of vanillin.
Perfumer Flavorist 31, 2836.
Fu, C., Tian, H., Li, Q., Cai, T., Du, W., 2006. Ultrasound-assisted extraction of
Fig. 8. Comparison of Ultrasound assisted extraction (time = 1 h) and conventional
xyloglucan from apple pomace. Ultrasonics Sonochemistry 13, 511516.
extraction methods (time = 8 h). Gogate, P.R., Shirgaonkar, I.Z., Sivakumar, M., Senthilkumar, P., Vichare, N.P., Pandit,
A.B., 2001. Cavitation reactors: efciency analysis using a model reaction.
American Institute of Chemical Engineers Journal 47, 25262538.
66.67 ml/g whereas ultrasonic assisted extraction required only Hromdkov, Z., Kotlov, Z., Ebringerov, A., 2008. Comparison of conventional
and ultrasound-assisted extraction of phenolics-rich heteroxylans from wheat
1 h for release of around 140 ppm vanillin concentration at similar
bran. Ultrasonics Sonochemistry 15, 10621068.
proportions of solvent to solute and under ambient operating tem- Kappatos, T., Gordon, M.H., Birch, C.G., 1996. Solution properties of vanillin and
perature. Similar increases using ultrasound has been reported in diaceteyl in aqueous ethanol solutions. Food Chemistry 57, 275282.
Ma, Y., Ye, X., Hao, Y., Xu, G., Xu, G., Liu, D., 2008. Ultrasound-assisted extraction of
the literature. Hromdkov et al. (2008) have reported that for sim-
hesperidin from Penggan (Citrus reticulata) peel. Ultrasonics Sonochemistry 15,
ilar yields of water-soluble polysaccharides from both extraction 227232.
steps and total isolated polysaccharides, ultrasonic irradiation re- Rao, R.S., Ravishankar, G.A., 2000. Vanilla avour: production by conventional and
quired 2% NaOH and 5 min of treatment time whereas classical biotechnological routes. Journal Science Food Agriculture 80, 289304.
Ranadive, A.S., 1992. Vanillin and related avor compounds in vanilla extracts made
process required about 80 min of time with 5% NaOH. Fu et al. from beans of various global origins. Journal of Agriculture Food Chemistry 40,
(2006) have also reported that ultrasound assisted extraction of 19221924.
xyloglucan was about three times faster than the traditional Rodrigues, S., Pinto, G.A.S., Fernandes, F.A.N., 2008. Optimization of ultrasound
extraction of phenolic compounds from coconut (Cocos nucifera) shell powder
extraction method. by response surface methodology. Ultrasonics Sonochemistry 15, 95100.
Romdhane, M., Gourdon, C., 2002. Investigation in solidliquid extraction: inuence
of ultrasound. Chemical Engineering Journal 87, 1119.
4. Conclusions
Sinha, A.K., Sharma, U.K., Sinha, N., 2008. A comprehensive review on vanilla avor:
extraction, isolation and quantication of vanillin and others constituents.
This study has enabled us to conrm the role of ultrasound in International Journal of Food Science Nutrition 59, 299326.
enhancing the rates of extraction by a comparison study with the Stanisavljevic, I.T., Lazic, M.L., Veljkovic, V.B., 2007. Ultrasonic extraction of oil from
tobacco (Nicotiana tabacum L.) seeds. Ultrasonics Sonochemistry 14, 646652.
conventional soxhlet extraction. In both the modes of extraction, Thompson, D., Sutherlands, D.G., 1955. Ultrasonic insonation effect on liquidsolid
the yield of vanillin in vanilla extract was higher for polar solvents extraction. Industrial Engineering Chemistry 47, 11671169.
such as ethanol and for higher proportion of solvent to solute. In Vinatoru, M., 2001. An overview of ultrasonically assisted extraction of bioactive
principles from herbs. Ultrasonics Sonochemistry 8, 303313.
the case of conventional soxhlet extraction use of higher operating Waliszewski, K.N., Pardio, V.T., Ovando, S.L., 2007. A simple and rapid HPLC
temperatures in the oil bath were found to give enhanced recovery technique for vanillin determination in alcohol extract. Food Chemistry 101,
of vanillin by virtue of higher rates of recycle for the solvent. Short 10591062.
Yang, Y., Zhang, F., 2008. Ultrasound-assisted extraction of rutin and quercetin from
period of pre-leaching was found to be effective enhancing the ex- Euonymus alatus (Thunb.) Sieb. Ultrasonics Sonochemistry 15, 308313.
tent of release of vanillin in the UAE by way of enhancing the per- Zhao, L.Q., Sun, Z.H., Zheng, P., Zhu, L.L., 2005. Biotransformation of isoeugenol to
meability of the cell wall. Compared with the conventional vanillin by novel strain of Bacillus fusiformis. Biotechnology Letters 27, 1505
1509.
extraction method (soxhlet), the UAE provided high extraction of