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Extraction of vanilla oleoresin (Vanilla planifolia Andrews) with supercritical CO2

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Actualmente la oleorresina de vainilla es uno de los productos naturales con alto uso. Su principal aplicación es como saborizante. En este trabajo se evalúa la extracción de oleorresina de vainilla usando CO2 supercrítico. Los principales parámetros variados para ver el efecto sobre el rendimiento y la concentración de vainillina fueron: presión, temperatura, tamaño de partícula, y tiempo de contacto. Obviamente los tamaños de particula menores favorecen la transferencia de masa y el mayor rendimiento de la oleorresina. Los valores mayores de presión y temperatura también dan mejores rendimientos de la oleorresina de vainilla. Las condiciones extremas de presión y temperatura reducen la calidad de la vainillina posiblemente debido a la degradación de algunos compuestos. La concentración más alta de vainillina (97.35% masa) se encuentra a una presión de 408 bar y a una temperatura de 40oC, con un rendimiento en masa de 5.82% con 40 minutos de extracción dinámica. La extracción de la vainilla con CO2 supercrítico es posible y la optimización de las condiciones de operación puede mejorar el rendimiento de la oleorresina con una buena concentración de vainillina. Para obtener el mejor tiempo de extracción es necesario realizar un análisis económico de factibilidad.
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Castillo-Ruz, María Carolina; Guillermo-Alcocer, Carlos Gerardo; Bojórquez-Gamboa,
Rubén Ricardo; Rocha-Uribe, José Antonio
Extraction of vanilla oleoresin (Vanilla planifolia Andrews) with supercritical CO2
Tecnología, Ciencia, Educación, vol. 26, núm. 2, julio-diciembre, 2011, pp. 80-84
Instituto Mexicano de Ingenieros Químicos
Distrito Federal, México
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80 Tecnol. Ciencia Ed. (IMIQ) vol. 26 núm. 2, 2011
Extraction of vanilla oleoresin (Vanilla planifolia
Andrews) with supercritical CO2
Tecnol. Ciencia Ed. (IMIQ) vol. 14 núms.1-2,1999 80Tecnol. Ciencia Ed. (IMIQ) 26(2): 80-84, 2011
*Autor a quien debe dirigirse la correspondencia
(Recibido: Junio 3, 2011,
Aceptado: Junio 29, 2011)
María Carolina Castillo-Ruz, Carlos Gerardo Guillermo-Alcocer, Rubén Ricardo Bojórquez-
Gamboa, José Antonio Rocha-Uribe*
Universidad Autónoma de Yucatán, Facultad de Ingeniería Química, Periférico Nte. Km 33.5 Tablaje Catastral 13615, Col.
Chuburná de Hidalgo Inn, 97203 Mérida, Yucatán; México. Tel. (Phone) (+52 999) 946 0981 Ext 1177; Fax 52 (999) 946 0994,
correo-e (e-mail): antonio.rocha@uady.mx
Extracción de oleorresina de vainilla (Vanilla
planifolia Andrews) con CO2 supercrítico
Palabras clave: CO2, extracción, uido supercrítico, vainilla,
vainillina, Vanilla planifolia Andrews
Keywords: CO2, extraction, supercritical uid, vanilla,
vanillin, Vanilla planifolia Andrews
ABSTRACT
Vanilla oleoresin is a widely used natural product, mainly used as avor.
In this work, the extraction of vanilla oleoresin using supercritical CO2
is evaluated. The main extraction parameters on the oleoresin yield and
composition was determined, namely: pressure, temperature, particle
size, and contact time. Results indicate that lower particle size favors
mass transfer and oleoresin yield. High pressure and temperature also
provide higher yields of vanilla oleoresin. Extreme conditions of pressure
and temperature decrease the quality of vanillin possibly because of
the degradation of some compounds. The maximum concentration
of vanillin (97.35% w/w) is found at 408 bars and 40oC, with a mass
yield of 5.82% after 40 minutes of dynamic extraction. The extraction
of vanilla oleoresin with supercritical CO2 is possible, and optimizing
the operational conditions may provide higher oleoresin yield with
good vanillin concentration; an economic analysis would be needed to
determine the best extraction time.
RESUMEN
Actualmente la oleorresina de vainilla es uno de los productos naturales
con alto uso. Su principal aplicación es como saborizante. En este trabajo
se evalúa la extracción de oleorresina de vainilla usando CO2 supercrítico.
Los principales parámetros variados para ver el efecto sobre el rendimiento
y la concentración de vainillina fueron: presión, temperatura, tamaño de
partícula, y tiempo de contacto. Obviamente los tamaños de particula
menores favorecen la transferencia de masa y el mayor rendimiento de
la oleorresina. Los valores mayores de presión y temperatura también
dan mejores rendimientos de la oleorresina de vainilla. Las condiciones
extremas de presión y temperatura reducen la calidad de la vainillina
posiblemente debido a la degradación de algunos compuestos. La
concentración más alta de vainillina (97.35% masa) se encuentra a una
presión de 408 bar y a una temperatura de 40oC, con un rendimiento en
masa de 5.82% con 40 minutos de extracción dinámica. La extracción de la
vainilla con CO2 supercrítico es posible y la optimización de las condiciones
de operación puede mejorar el rendimiento de la oleorresina con una buena
concentración de vainillina. Para obtener el mejor tiempo de extracción es
necesario realizar un análisis económico de factibilidad.
INTRODUCTION
Vanilla (Vanilla planifolia Andrews) is native from
southeastern Mexico and is considered the world’s main
avor (Brandt, 1996, Havkin-Frenkel y Belanger, 2011).
The rst component of vanilla aroma is vanillin, which
is obtained from a natural fermentation process known
as curing. According to Ranadive (1992), since most
of the components that provide the avor are volatile
and thermolabile, extraction and purication methods
of vanilla extracts determine the overall quality of the
nal product. Presently, the main extraction method for
vanilla oleoresin is multistage lixiviation, or leaching at
80oC employing ethyl alcohol, but if the process does
not have a good control of temperature, degradation of
vanilla may occur and a loss of extract exists.
Supercritical extraction with CO2 seems to be a good
alternative, because it operates at a lower temperature,
mass transfer is improved, and no residual solvent
Tecnol. Ciencia Ed. (IMIQ) vol. 26 núm. 2, 2011 81
is present in the nal product. These advantages are
important and seem promising for the industrial use
of this technology in the extraction of thermolabile
compounds (Moyler and Heath, 1988).
Moyler (1987) reviews the sub- and supercritical
CO2 extraction of essential oils and compare results
with steam distillation for ginger, hop, clove bud,
black pepper, juniper berry oil, and vanilla bean. Rice
and Singh obtained a patent in 1990 for the continuous
extraction of solid material using solvents such as CO2
by circulating a mixture of the solids in CO2 at elevated
pressure through a closed-loop pipeline. Carbonell
(1991) reviews extraction with CO2 of ginger, black,
green, and white pepper, and vanilla. Fu et al. (2002a,b),
report the extraction of vanilla with supercritical CO2
fluid. Kvasenkov and Kvasenkov (2010) patented
the preparation of coffee-substitute beverages using
supercritical extraction of a mixture of cocoa husk,
cinnamon and vanilla spices with liquid nitrogen.
The objective of this research is to evaluate the yield
and nal concentration of vanilla oleoresin extracted
by supercritical CO2. A study of the effect of pressure,
temperature, particle size, and contact time is also
included.
MATERIALS AND METHODS
Materials
The raw materials were vanilla beans from Papantla,
Veracruz, Mexico (from Casa Larios). The vanilla
beans were classied as superior quality based on the
parameters accepted in Mexico (Mexican Act NMX-
FF-074-1996). The content of vanillin in the vanilla
beans was determined according to the same norm. The
traditional extraction procedure consists of maceration
of vanilla beans cut to about 0.65 cm on ethanol.
Total vanillin content was 3.6% w/w after 3 days of
maceration time. The extraction yield is dened as
grams of oleoresin extracted and recovered divided by
the grams of solid material in the extraction recipient.
The concentration of vanillin was characterized by
HPLC as recommended by Thomson and Hoffmann
(1988). Yield and composition obtained in this research
are compared against the values reported by Nguyen et
al. (1991).
Solvents
The solvent was industrial-grade CO2 at 99.98% w/
w, supplied by Praxair-Mexico. Other reactants and
solvents were purchased from Merck (Mexico). Vanillin
standard with 99% purity was supplied by Sigma-
Aldrich (Mexico).
SUPERCRITICAL EXTRACTION
Equipment
The supercritical extraction of vanilla oleoresin was
performed with lab-scale equipment (model SFT-150
System Extractor from Supercritical Fluid Technologies,
Inc. Newark, DE, USA) A typical diagram is shown in
Figure 1. The capacity of the extraction cell is 0.1 L
and usually was charged with 23 g of vanilla beans.
The equipment has an air-driven reciprocating pump
to compress the CO2. The heating elements are 2000
W resistances and a temperature proportional integral
derivative (PID) controller allows xing the temperature
in the range from 0 to 120oC. The ow of CO2 is
between 1 and 330 mL/min (1-250 g/min) of liquid CO2
under normal operation.
Operational conditions
Table 1 shows the operational conditions studied in
the experimental runs (data obtained by triplicate) and
reported by Castillo-Ruz (2007). The temperature and
pressure range is wider than that reported by Nguyen
et al. (1991). The extractions were performed at 40,
45, and 50ºC, and at four different pressures 272,
Figure 1. Extraction system using supercritical
CO2: A. Air cylinder (T-1) and CO2
cylinder (T-2); B. Manometer for air
(M-1 y M-2); C. Cooler for liquid CO2
(IC-1); D. Reciprocant pump (B-1); E.
Regulatory valve for air fed to pump
(V-5); F. Extractor (E-1); G. Valve
on/off (V-6); H. Needle valve (V-7); I.
Containers: Extractor (E-2) solvent
trap (E-3); J. Flow meter (R-1)
M-1
M-2P
P
T-1 T-2
A la atmósfera
R-1
E-3
E-1
E-2
G H
V-6
V-8
V-2
V-1
V-4
V-3 V-5
V-7
I
J
F
D
C
E
B
IC-1
B-1
A
82 Tecnol. Ciencia Ed. (IMIQ) vol. 26 núm. 2, 2011
340, 408, and 476 bar (4000, 5000, 6000, and 7000
psi, respectively). The particle size was between
16 and 30 μm for most of the runs. One of the runs
included vanilla beans pieces of 5 mm in length as a
reference. Particle size was detemined with standard
sieves(Newark, US). For most of the runs, contact
time was 40 minutes, but for each pair of pressure and
temperature contact times of 30 and 60 minutes were
also tested to see the effect of these variables.
Table 1
Summary of the operational conditions used
in the experimental data to be obtained from
the temperature dependent design for vanilla
supercritical extraction
Temperature, °C
40 45 50
Pressure (bar)
272.11 272.11 272.11
340.14 340.14 340.14
408.16 408.16 408.16
476.19 476.19 476.19
For each supercritical extraction run with CO2 the
yield was calculated as follows:
yield = ––––––––––––––––––––––––––––––––
grams of vanilla oleresin extracted
grams of vanilla charged to extraction cell (1)
Extraction procedure
Referring to Figure 1, at the beginning of the extraction
the on/off valve (V-6) is closed and valves V-2 and V-4
for liquid CO2 are opened. The extraction cell (E-1)
is lled with 23 g of vanilla beans, closed, and xed.
The desired temperature set point is set on the PID
controller. The pressure is gradually increased by using
the regulatory valve V-5 until the desired pressure is
obtained. The soaking time starts once the operational
conditions for temperature and pressure are established;
this takes 15 minutes, and during this lapse there is no
ow of CO2 to the extraction cell. After the soaking
time, CO2 is allowed to ow by opening the on/off
valve (V-6); then the supercritical CO2 ows upwards
through the solid matrix of vanilla beans, extracting
the oleoresin both from the pores and the outer part of
the bean particles, diffusing out along with the CO2.
The extract is collected in the container (E-2), where
the CO2 de-pressurization occurs down to atmospheric
conditions. The continuous extraction process takes
40 minutes. The decompressed gaseous CO2 leaves
the container (E-2) and enters a second container (E-3)
which is immersed in ice. The purpose of this second
container is recovering the extract that may remain
dissolved in the gaseous CO2. The ow used for the
dynamic extraction period is measured with a ow meter
(R-1) before CO2 is discarded to the atmosphere. The
CO2 ow is regulated with a needle valve (V-7). When
the dynamic extraction period ends, valves V-1, V-2,
V-3, and V-4 are closed, and valve V-6 is opened. Then
the extraction cell (E-1) is de-pressurized, the remaining
solid matrix and the collected extract are weighed, a
mass balance is performed, and the oleoresin yield is
calculated with Equation 1.
HPLC analysis
Identication and quantication of vanilla in the extracts
was carried out by liquid chromatography (Perkin
Elmer 250) with a binary pump and a UV absorbance
detector at 275 nm. For the chromatographic separation,
an analytic column Spherisorb ODS2 was used. For
identication and quantication of vanillin, a standard
with 99% purity was obtained from Sigma-Aldrich
(Mexico).
RESULTS AND DISCUSSION
Effect of particle size on the yield of vanilla
oleoresin
Preliminary extractions at 272 bar (4000 psi) and
50oC using the 5 mm and 16-30 µm particle sizes,
were performed. As expected, the yield (4.95%) for
the smaller matrix (16-30 µm) is higher than the yield
(1.5%) for vanilla beans cut at 5 mm, confirming
that smaller size favors mass transfer of solute to the
supercritical CO2, because of a larger transfer surface-
area, according to Fick’s law. Therefore, all the other
runs were performed using the smaller particle size
(16-30 µm).
Effect of temperature and pressure on the
oleoresin yield
Figure 2 show the oleoresin yields obtained at different
pressure and temperature with a dynamic time of 40
minutes.
A general tendency of higher yields for higher
temperature and pressure conditions is observed. It seems
that pressure increments provide higher oleoresin yields.
A maximum yield of 7.77% is found for 50oC and 476.19
bar for an extraction time of 40 minutes, for grinded
vanilla beans (16-30 µm). Nguyen et al (1991) reported
Tecnol. Ciencia Ed. (IMIQ) vol. 26 núm. 2, 2011 83
yields from 0.3 to 8.0%, using a lower temperature range
(33-36oC) and lower operational pressure (110 bar), as
well as an average particle thickness of 1.8 mm, average
width of 4 mm and average length of 19 mm, and higher
extraction times (5-1540 h). These authors also report
experimental data for 110 bars, 36oC with cryoground
vanilla with a yield of 10.6% for a time of 50 hours.
Yields obtained in this research are higher than those
reported by Nguyen et al (1991), with a lower extraction
time. The reasons in order of importance from low to
high are:
a. Higher temperature (40-50 vs. 33-36oC)
b. Higher pressure (272-476 vs. 110 bar)
c. Lower particle size (0.023 vs. 19 mm)
Identication of vanillin on oleoresin
Once the yield of oleoresin was measured, the oleoresin
was analyzed for vanillin and other compounds by
liquid chromatography as recommended by Thompson
and Hoffmann (1988). Retention time for vanillin
was 7 minutes. Depending upon temperature and
pressure conditions used on the extractions, other
compounds that contributed for the vanilla oleoresin
bouquet were found. For example, on the performed
extract chromatograms (272 bars and 50oC) a peak at
2.59 minutes of retention time was observed, which
corresponds to p-hydroxybenzoic acid.
Effect of temperature and pressure on vanillin
concentration
Figure 3 shows the percentages of vanillin, measured
on the extracts by using HPLC analyses. Considering
the pressure and temperature that provided the
maximum percentage of vanillin, it was found that
intermediate pressure values between 340 and 408 bar,
and temperatures around 40 and 45oC favor vanillin
concentration. The maximum mass concentration of
vanillin (97.35%) is found at a pressure of 408 bars and
a temperature of 40oC.
Figure 2. Yield of vanilla oleoresin expressed on
mass percentage at 40, 45, 50ºC
Effect of contact time
Figure 4 shows the effect of dynamic extraction time.
As expected, there is a higher extraction yield for longer
times. It is observed that, mainly for higher pressures,
from 30 to 40 minutes the increment in the yield is about
double than the increment from 40 to 60 minutes.
Using an extraction time of 40 minutes leaves solute
in the solid matrix. Working at extraction times of 60
minutes the recovery of solute is a little higher. For
industrial extraction, an economical analysis would be
needed to determine the optimum extraction time.
Figure 4. Effect of extraction time over oleoresin
yield (30, 40, 60 min)
8
7
6
5
4
3
2
1
0
272.11 340.14 408.16 476.19
Pressure (bar)
Yield
40
40 40 40
45 45
45
45
50
50 50
50
Figure 3. Mass percentage of vanillin at different
operation conditions (40, 45, 50 ºC)
100
90
80
70
60
50
40
30
20
10
0
272.11 340.14 408.16 476.19
Pressure (bar)
40 40
40
40
45
45
45
45
50
50
50 50
84 Tecnol. Ciencia Ed. (IMIQ) vol. 26 núm. 2, 2011
CONCLUSIONS
From this research the following conclusion may be
drawn:
Lower particle size favors mass transfer and oleoresin
yield, higher pressure and temperature also provide
higher yields of vanilla oleoresin.
Extreme conditions of pressure and temperature
decrease the quality of vanillin, possibly due to
degradation of some compounds. The maximum
concentration of vanillin (97.35% w/w) is found at a
pressure of 408 bars and a temperature of 40oC, with
a mass yield of 5.82% after 40 minutes of dynamic
extraction.
The extraction of vanilla with supercritical CO2 is
possible and optimizing the operational conditions may
provide higher oleoresin yields with a good vanillin
concentration.
An economical analysis is needed to determine the
optimum extraction time.
ACKNOWLEDGMENTS
The authors would like to acknowledge the valuable
support of:
i. Dr. Juan-Daniel Pacho-Carrillo and Dra. Rosa-
María Domínguez-Espinoza
ii. Dr. Julio C. Sacramento Rivero
iii. PRIORI Program (Program of Impulse and
Orientation to Research, Spanish acronym),
Autonomous University of Yucatan, Mexico
iv. Multimarcas y Servicios de México, S.A.
v. The experimental work was performed at the
Faculty of Chemical Engineering, Autonomous
University of Yucatan, Mexico. It was reported as
the professional thesis of María Carolina Castillo-
Ruz (2007).
NOMENCLATURE
HPLC High performance liquid chromatography
PID Proportional integral derivative controller
BIBLIOGRAPHY
Brandt, L. 1996. The creation and use of vanilla. Food Product Design
Magazine. March 01. Available from http://www.foodproductdesign.com
Carbonell, E. S. 1991. Extraction of avors with supercritical carbon
dioxide. Cereal Foods World. 36(11):935-937.
Castillo-Ruz, M. C. 2007. Extracción de oleorresina de vainilla (Vanilla
planifolia Andrews) con CO2 supercrítico . Tesis profesional.
Industrial Chemical Engineering, Universidad Autónoma de Yucatán.
Mérida, Yucatán, México.
Fu, S., Huang, M., Zhou, J., Li, S. 2002a. Determination of chemical
constituents of vanilla by supercritical CO2 uid extraction. Huaxue
Yanjiu Yu Yingyong. 14:208-210.
Fu, S., Huang, M., Zhou, J., Li, S. 2002b. Study of components of vanilla
extract by different extracting technology. Shipin Kexue. 23:109-112.
Havkin-Frenkel, D., Belanger, F. 2011. Handbook of Vanilla Science and
Technology. Wiley-Blackwell. Nueva York, NY. EEUU.
Kvasenkov, O. I., Kvasenkov, I. I. 2010. Method for production of coffee
drink “Rossiiskii”. Russian Patent RU 2402914 C1. Moscú, Rusia.
Mexican Act NMF-FF-074-1996: Food products not industrialized for human
consumption – species and condiments –entire and dry vanilla (Vanilla
fragrant Salisbury Ames o Vanilla planifolia Andrews). Diario Ocial de
la Federación. Estados Unidos Mexicanos. Mexito City, Mexico.
Moyler, D. A. 1987. Liquid carbon dioxide extraction of avor materials. En
Dev. Food Flavours [Industrial Co-op Symp.], pp. 119-29. Conference.
General review 1986. Elsevier Appl. Sci. Londres, Reino Unido.
Moyler, D. A., Heath, B. 1988. Liquid carbon dioxide extraction of essential
oils. Flavors and fragrances: A world perspective. En Proceedings of
the 10th International Congress of Essential Oils, Fragrances and
Flavors. Pp. 41-63. Elsevier. Londres, Reino Unido.
Nguyen, K., Barton, P., Spencer, J. 1991. Supercritical carbon dioxide
extraction of vanilla. The Journal of Supercritical Fluids. 4(1):40-46.
Ranadive, A. S. 1992. Vanillin and related avor compounds in vanilla
extracts made from beans of various global origins. J. Agric. Food
Chem. 40:1922-1924.
Rice, W.K., Singh, L. 1990. Dynamic supercritical uid extraction system,
US Patent No. 4898673 A. Washington, DC. EEUU.
Thompson, R. D., Hoffmann, T. J. 1988. Determination of coumarin as an
adulterant in vanilla avoring products by high performance liquid
chromatography. Journal of Chromatography. 438:369-382.
... Despite the information made available through studies of supercritical vanilla extraction (Castillo-Ruiz, Guillermo-Alcocer, Bojórquez-Gamboa, & Rocha-Uribe, 2011;Fang, Shi, & Zhang, 2002;Nguyen, Barton, & Spencer, 1991;Romero-de la Vega, Salgado-Cervantes, García-Alvarado, Romero-Martínez, & Hegel, 2016), little is known about volatile compounds other than vanillin in vanilla oleoresins. The concentrations of volatile compounds present after a time of half the one used during traditional have not been evaluated, and the composition of fatty acids in vanilla oleoresins has not been determined. ...
... The oleoresin yields ranged from 2.12% to 4.95% (w/w) ( Figure 1), and the maximum yield was obtained from SFE performed at 20 MPa and 40°C. These values were consistent with those reported in previous studies (Castillo-Ruiz et al., 2011;Nguyen et al., 1991). Generally, oleoresin yield increased as the pressure and temperature were increased. ...
... Nguyen et al. (1991) reported yields ranging from 0.3% to 8.0% (w/w) with extraction temperatures from 33°C to 36°C at a pressure of 11.0 MPa. Castillo-Ruiz et al. (2011) obtained yields between 4.0% and 7.77% (w/w), and their maximum yield was obtained from extraction at 476.19 MPa and 50°C. On the other hand, Naik et al. (2014) reported a yield of 3.2% (w/w) from extraction at 30 MPa and 50°C. ...
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Vanilla is one of the most popular species in the world. Its main compound, vanillin, is responsible for its characteristic aroma and flavor and its antioxidant and biological properties. Vanillin is very unstable in the presence of oxygen, light, and humidity, which complicates its use and preservation. Therefore, to solve this problem, this study aimed to develop vanilla oleoresin microcapsules. Vanilla oleoresin was obtained with supercritical carbon dioxide and microencapsulated by complex coacervation and subsequent spray drying (100 °C/60 °C inlet/outlet temperature). The optimal conditions for the complex coacervation process were 0.34% chitosan, 1.7% gum Arabic, 5.29 pH, and an oleoresin:wall material ratio of 1:2.5. Fourier Transform Infrared Spectroscopy (FT-IR) analysis of the coacervates before and after spray drying revealed the presence of the functional group C=N (associated with carbonyl groups of vanillin and amino groups of chitosan), indicating that microencapsulation by complex coacervation-spray drying was successful. The retention and encapsulation efficiencies were 84.89 ± 1.94% and 69.20 ± 1.79%. The microcapsules obtained from vanilla oleoresin had high vanillin concentration and the presence of other volatile compounds and essential fatty acids. All this improves the aroma and flavor of the product, increasing its consumption and application in various food matrices
Book
Vanilla is the world's most commonly-used flavour and fragrance, used in foods, cosmetics, pharmaceuticals and other products and is therefore of considerable economic importance. This book provides a comprehensive overview of the science and technology used in the production and supply chain of vanilla products. A wide range of international authors cover topics which include agricultural production, global markets, analytical methods, sensory analysis, food and fragrance applications, organic and fair trade vanilla, diseases that affect vanilla, and novel uses. It is of interest to academic researchers in this field and is also an important resource for the vanilla industry and those companies that use vanilla and vanillin as flavours and fragrances worldwide. Key Features: • The only book to cover such a wide range of topics on this most commercially valuable of flavour ingredients • Includes an analysis of the current vanilla markets in the US and Europe • Edited by experts who hold roles in the flavour industry and academic research.
Article
Extraction using supercritical fluids in particular carbon dioxide is a process that has become increasingly significant over the post decade in pharmaceuticals, cosmetics, food processing and beverages industry. Supercritical carbon dioxide is a particularly good solvent and has the added advantage of being physiologically harmless. In this application it has absolutely no residue problems. Further advantages of using supercritical carbon dioxide extraction are inert atmosphere during processing and the possibility of selective extraction.
Article
Oleoresin was extracted from vanilla beans with 2–62 g CO2/g dried bean at 306–309 K and 10–13 MPa. Effects of extraction time (5 to 1540 h), water-soaking of beans, and cryogrinding of beans on oleoresin yield and composition were determined. Vanillin yields up to 95% were attained. Extraction rate was first-order with respect to unextracted oleoresin concentration. Vanillin purity was higher with supercritical C02 extraction than with conventional aqueous ethanol extraction; the vanillin represents 74–97% of the flavor and fragrance compounds, measured by liquid chromatography, when using CO2 compared to 61 % using alcohol extraction.
Article
Vanilla beans from seven different vanilla growing regions of the world were analyzed for vanillin, p-hydroxybenzoic acid, p-hydroxybenzaldehyde, and vanillic acid. Beans were extracted to obtain singlefold extracts, and analysis was carried out using reversed-phase liquid chromatography. Analysis of the extracts, obtained from cured and uncured beans treated with beta-glucosidase, indicates that all of the above-mentioned compounds are present in green beans as glycosides and are released upon curing. In addition to glycosides of these four known monophenols, there are at least three other major glycosides in green vanilla beans which are hydrolyzed during the curing process.
Article
A high-performance liquid chromatographic procedure was developed for the isolation and quantitation of coumarin from vanilla-based liquid flavorings of Mexican origin. Forty products representing fourteen different Mexican brands were assayed for coumarin, vanillin, and ethyl vanillin by the proposed method. The procedure has been adapted to the analysis of other products including domestic vanilla extracts and imitation vanilla flavorings for vanillin, ethyl vanillin, 4-hydroxybenzaldehyde and piperonal. Chromatographic retention data for thirty-seven compounds associated with vanillin and vanilla products employing two mobile phase systems are presented.
Method for production of coffee drink " Rossiiskii " . Russian Patent RU 2402914 C1
  • O I Kvasenkov
  • I I Kvasenkov
Kvasenkov, O. I., Kvasenkov, I. I. 2010. Method for production of coffee drink " Rossiiskii ". Russian Patent RU 2402914 C1. Moscú, Rusia.
Determination of chemical constituents of vanilla by supercritical CO 2 fluid extraction
  • S Fu
  • M Huang
  • J Zhou
  • S Li
Fu, S., Huang, M., Zhou, J., Li, S. 2002a. Determination of chemical constituents of vanilla by supercritical CO 2 fluid extraction. Huaxue Yanjiu Yu Yingyong. 14:208-210.
The creation and use of vanilla. Food Product Design Magazine Available from http://www.foodproductdesign.com Carbonell, E. S. 1991. Extraction of flavors with supercritical carbon dioxide. Cereal Foods World
  • L Brandt
Brandt, L. 1996. The creation and use of vanilla. Food Product Design Magazine. March 01. Available from http://www.foodproductdesign.com Carbonell, E. S. 1991. Extraction of flavors with supercritical carbon dioxide. Cereal Foods World. 36(11):935-937.
Liquid carbon dioxide extraction of essential oils. Flavors and fragrances: A world perspective
  • D A Moyler
  • B Heath
Moyler, D. A., Heath, B. 1988. Liquid carbon dioxide extraction of essential oils. Flavors and fragrances: A world perspective. En Proceedings of the 10th International Congress of Essential Oils, Fragrances and Flavors. Pp. 41-63. Elsevier. Londres, Reino Unido.
Dynamic supercritical fluid extraction system, US Patent No. 4898673 A
  • W K Rice
  • L Singh
Rice, W.K., Singh, L. 1990. Dynamic supercritical fluid extraction system, US Patent No. 4898673 A. Washington, DC. EEUU.