2nd Mercosur Congress on Chemical Engineering

4th Mercosur Congress on Process Systems Engineering

EXTRACTION OF THE INULINE FROM CHICORY ROOTS

(Chicorium intybus L.) USING SUPERCRITICAL CARBON DIOXIDE
Marisa F. Mendes1*, Luana F. Cataldo2, Cristiano A. da Silva2, Regina I. Nogueira3, Suely P. Freitas2
1
Pesquisadora CNPq - DEQ - Universidade Federal Rural do Rio de Janeiro
2
Escola de Química - Universidade Federal do Rio de Janeiro
3
EMBRAPA – CTAA

Abstract. The chicory, tuberous roots that store inulin, is a native plant from Europe, Asia, Africa and South
America but it can be cultivate in all over the world. The inuline is a polysaccharide that can be found in a
series of vegetable products like chicory roots (Chicorium intybus L.). It is mostly used in the food industry
for production of low caloric foods, acting as a substitute of sugar or fat. The inuline is also utilized as a
functional ingredient in the food and pharmaceutical industries. The conventional technology used to produce
inuline is the aqueous extraction, but the energetic costs of this process are very high due to the presence of
separation steps including filtration, evaporation and drying using spray-dryers. Considering that Brazil is
recognized as the most active country in Latin America involved in supercritical CO2 R&D and the other
hand, does not have a commercial production of inuline, the motivation of this work is evaluate the
operational parameters of supercritical extraction technology of inuline from chicory. Extractions were done
in an experimental apparatus containing a stainless steel extractor, a micrometer valve, a high-pressure pump
and a heating bath. Approximately 16 grams of crushed chicory was fed to the extractor. The experimental
conditions has been investigated the effect of temperature in the range of 40 to 80ºC and pressure in the range
of 62 to 170 bars in an operational time of 2 hours. The maximum solute recovery was reached at 40ºC and
150 bars, for 2 hours of extraction. As occurred in many supercritical processes, the experimental results
indicated that when the pressure is increased, the extracted mass increases at constant temperature and when
the temperature increased at constant pressure, the extracted mass decreases due to the decrease of the solvent
density.

Keywords: Carbon Dioxide, Inuline and Chicory.

1. Introduction

The chicory (Cichorium intybus) is a tuberous roots that store inuline, a fructan polysaccharide, of degree of
polymerization 11–60 and composed with a high fructose content (about 94%) and a terminal glucose molecule.
It is common known that fructose has got a higher sweetening power than glucose or sucrose and, unlike such
sugars, can be used also by diabetic people. It acts in the organism in a similar way to dietary fibers, contributing
to the improvement of the gastrointestinal system conditions. Due to these properties, food and pharmaceutical
industries have found applications for inulin in the production of functional foods, nutritional composites and
medicines (Figueira et al., 2004). The chicory roots can be seen in Figure 1.
Most of the industrial production of fructose is actually obtained from corn starch as a fructose-rich syrup
(isoglucose) by an enzymatic hydrolysis process, followed by glucose isomerisation and subsequent fructose
separation. Recover fructose directly from crops that can synthesis and accumulate large amounts of such sugar
polymers would be a more attractive industrial possibility.
Fructose syrup extracted from roots of chicory is nowadays produced on an industrial scale only by few
industries in northern and central European countries (Belgium, the Netherlands, France). The conventional

*
To whom all correspondence should be addressed.
Address: DEQ/IT/UFRRJ – BR 465 – Km 7, Seropédica – Brazil

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4th Mercosur Congress on Process Systems Engineering

technology used to produce inuline involves the following steps: liquid extraction, filtration, evaporation and
spray drying. The energetic costs of this process are very high due to the concentration and drying stages
(Nogueira, 2002).

Fig. 1. Chicory roots

Sustainable development has become a key ideal at the 21st century. To reach environmental, economic and
social objectives scientists will be confronted to very demanding tasks. They must develop new processes,
environmentally acceptable with minimum consumption of energy and raw materials, also maintaining an
ecological balance as favorable as possible. Supercritical fluid extraction, using carbon dioxide (CO2) as solvent,
is a clean technology actually recommended for different applications in food industries. This solvent is not only
cheap and readily available, but also safe to handle. Furthermore, CO2 is easily removed by simple expansion to
environmental pressure values and consequently it is approved for food processing without declaration (Brunner,
2004).
Del Valle et al. (2005) reviewed the application of high pressure carbon dioxide in Latin America. According
to this review, Brazil is the most active country in Latin America due to networking initiatives to research and
development. The modeling of the supercritical fluid extraction process for scaling-up purposes and evaluation of
the technical and economical feasibility of some selected processes would allow a successful regional
implementation of this technology. Considering that Brazil does not have a commercial production of inuline and
its favorable conditions to installation of a supercritical CO2 extraction plant, the objective of this work is to
evaluate the operational parameters and profitability of this technology to inuline extraction from chicory roots.

2. Materials and Methods

E-mail: mf_mendes@hotmail.com
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4th Mercosur Congress on Process Systems Engineering

2.1. Materials
The chicory roots was supplied by Embrapa Agroindústria de Alimentos and CO2 (99.9% of minimum purity)
by AGA S.A. The extraction of inuline was initially done in a semi-batch process. The laboratory apparatus
consists of an extractor with an internal volume of 42 ml, made of stainless steel 316L. Canvas with stainless
steel of 260 mesh were joined in each edge of the extractor to prevent the loss of material. The micrometric valve
(Whitey, model SS-31RS4), located downstream the extractor, is used to control the flowrate. The raffinate was
recovered in a buret and the flowrate of the solvent was measured in the rotameter.
The operation pressure of the equipment is reached through a high pressure pump (Thermo Separation
Products, Constametric 3200 P/F) that feeds the carbon dioxide. The specifications of pressure and flowrate of
the high pressure pump was 400 atm and 9.99 ml/min. A schematic view of equipment is showed in Figure 2.
The experimental apparatus was previously tested and validated in Mendes (2002).

2.2. Experimental Methodology

The extractor was fed with a known quantity of chicory roots and then, the experimental procedure initializes
turning up the heating bath to heat the extractor to the desired temperature. After the desired temperature is
reached, CO2 is supplied to the extractor by action of a high-pressure pump at 9.83 ml/min. A bath with ice and
salt (temperature equal to –10ºC) was maintained in the pump inlet to guarantee the liquid state of carbon
dioxide. The extractions were performed at 40, 60 and 80ºC and 62, 100, 150 and 170 bars. The operational time
was fixed in 2 hours.

2.3 Statistical Analysis

A factorial design (32), three level two parameter, was proposed to analyze the effect of the temperature and
pressure on extract mass (table 1). The statistical calculations were carried out by variance analysis using the
Statistica Software (1997). The probability (p) values were used as a tool to check the statistical significance of
each independent variable (Barros Neto, 1996).

Table 1. Independent variables and experimental design levels

Variables levels

Independent variables -1 0 +1

Temperature (oC) 40 60 80

Pressure (bar) 100 150 170

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Fig. 2. Experimental apparatus used to study the extraction of inuline from the chicory roots, where A – gas
cylinder, B – high pressure pump, C – heating baths, D – extractor, E – micrometer valve, F – raffinate, G –
rotameter.

3. Results and Discussions

Approximately 14 to 15 g of chicory roots are fed into the extractor and due to these differences, the extract
mass can varies for each operational condition. The extraction yield was calculated by the ratio between the
extract mass and the sample mass, knowing that the initially inuline concentration in the chicory is around 12.8 to
15.8 for each 100g of raw material. To better explain the behavior of the experimental results, the S/F ratio
(solvent/feed) was calculated based on the flow rate of the solvent (9.83 ml/min), the batch time of 2 hours and
the density of the carbon dioxide for each operational condition of temperature and pressure.
As it can be observed in Fig 3, at constant temperature, the yield increases as pressure increases, due to the
increase of the carbon dioxide density at constant temperature. This occurs because the solvent power of the
solvent always increases. However, the increase in temperature promotes the slightly decrease in the yield due to
the decrease of the solvent density, at constant pressure.
In general, as the S/F ratio increases the mass of extract increase. However this is not observed for all
operational conditions investigated (Fig. 4). The initial slope in this plot represents the ‘‘operational’’ solubility
of inulin in SC-CO2.
Analyzing the temperature behavior, at constant pressure, it can be observed that the yield decreases at 60ºC,
for all the pressures investigated, in comparison to 40ºC; but at 80ºC, the yield is higher than at 60ºC. The first
behavior is expected because the density of CO2 decreases with the increase of the temperature, decreasing the
solvent power of the solvent. This behavior was not observed when the temperature increases from 60 to 80ºC. It
occurs because when the temperature increases, at constant pressure, the vapor pressure of the solvent also
increases, increasing the extracted mass, balancing the effect of the decrease in the solvent density.
At pressures of 150 and 170 bars, the yield decreases when the temperature increases from 40 to 60ºC and
from 60 to 80ºC.

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As can be observed from Pareto chart (Fig. 5), pressure is a significant parameter at 85% of confidence level
(p<0.15). However, the extract mass are not statistically influenced as temperature increase of 40 to 60oC.
Response surface plots generated (Fig. 6) shows that the better extraction (0.008 g of extract) is reached at
pressure equal to 150 bar. As pressure increase to 170 bar, the extract mass decrease to 0.006 g

Table 2. Results of the inulin extractions by SC-CO2, performed at different operational conditions

Pressure (bar) Sample mass (g) Extract mass (g) Yield (%) S/F (kg CO2/kg sample).

T=40ºC
62* 14.6854 0.0032 0.0221 12.1266
100 15.0007 0.0058 0.0396 48.9008
150 15.4479 0.0069 0.0453 59.8957
170 15.1642 0.0062 0.0407 63.6013

T=60ºC
62* 15.0254 0.0023 0.0157 10.353
100 14.8906 0.0050 0.0336 23.428
150 15.3199 0.0088 0.0570 46.99
170 15.2154 0.0072 0.0473 51.4917

T=80ºC

62* 14.411 0.0065 0.0459 9.4765

100 15.013 0.0066 0.0436 17.5516
150 15.3242 0.0069 0.0448 33.437
170 14.2115 0.0062 0.0439 38.7723

* cylinder pressure

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0.06

0.05

Total Efficiency (%)

0.04

0.03

40ºC
0.02
60ºC
80ºC

0.01

40.00 80.00 120.00 160.00 200.00

Pressure (bar)

Fig. 3. Total yield in function of different conditions of pressure, at the temperatures of 40, 60 and 80ºC

0.06

0.05
Total Efficiency (%)

0.04

0.03

40ºC
0.02
60ºC
80ºC

0.01

0.00 20.00 40.00 60.00 80.00

Kg CO2 / Kg sample

Fig. 4. Yield in function of the S/F ratio, at 40, 60 and 80ºC

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2 3-level factors, 18 Runs; MS Residual=.0000008

DV: extract mass (g)

pressure (bar)(Q) 1.835661

(1)pressure (bar)(L) 1.029965

Temperature ( oC)(Q) .7497772

(2)Temperature ( oC)(L) .5821544

p=.15
Effect Estimate (Absolute Value)

Fig 5. Pareto Chart of Standardized Effects; Dependent Variable: inulin extract mass (g)

Fitted Surface; Variable: extract mass (g)

2 3-level factors, 18 Runs; MS Residual=.0000008
DV: extract mass (g)

Extract
mass (g)

0.0075
0.007
0.0065
Temperature (ºC) Pressure (bar) 0.006
0.0055

Fig 6. Effect of pressure and temperature and their interaction on extract mass of inulin

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4. Conclusions and Suggestions

The objective of this work was the inuline extraction using the supercritical fluid technology. The operational
conditions studied varied from 40 to 80ºC and from 62 to 170 bars. The better result of the extraction was at
60ºC and 150 bars. This behavior was also confirmed in the statistical analysis. It was observed that the results at
the temperature of 80ºC were not influenced by the pressure increase.
The efficiency of inulin extraction by SC-CO2, measured by relation between extracted mass and inulin mass
present in the raw material, is inferior to 10%, probably due to high molecular weight of inulin, a carbohydrate
polymers consisting of a sucrose molecule that is elongated by a chain of fructosyl units connected. To increase
the efficiency of inuline extraction, a co-solvent could be used with the carbon dioxide.

References

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