A Novel Technique for the

Decolorization of Sugarcane Juice

M. OKUNO AND H. TAMAKI

ABSTRACT: A novel technique for the decolorization of sugarcane juice has been developed. In this method, the
coloration caused by polyphenols during the refining of cane sugar was removed by treatment with octadecylsilylsilicagel. The efficiency of color removal was nearly 90%.
Keywords: sugarcane juice, polyphenols, octadecylsilyl-silicagel, decolorization

Introduction

RODUCED IN PROCESSING SUGAR , SUGARCANE JUICE CON -

Food Engineering and Physical Properties

tains a variety of polyphenols, such as flavonoids (Paton

and others 1985; Smith and Paton 1985), phenolic acids (Paton 1992), phenolic glucosides (Palla 1982), and phenylpropanoids (Nakasone and others 1996). These compounds are
the main source of colorants, essentially considered impurities. Removal of these polyphenols is generally done by using
bone char. However, newer factories are currently using ionexchange resins because bone char regeneration is costly.
Due to the difficult regeneration process for high-color sugar
syrups by ion-exchange resins, many studies on the effective
regeneration of these resins have been done (Bento 1997;
Bento 1998). Furthermore, since much brine/caustic liquid
waste is discharged when ion-exchange resins are regenerated, efforts have been made to reduce these various wastes
(Stacey and John 1997).
Octadecylsilyl-silicagel (ODS) is widely used in reversephase chromatography as a strong adsorbent of polyphenols. ODS can be regenerated by using alcohol, which can
easily be recovered by evaporation. Hence, if ODS is used as
the decolorizer of sugarcane juice, no liquid wastes will be
produced from the clarification system.
The objective of this study was to decolorize sugarcane
juice by removing polyphenols with ODS adsorption, then
recover these important polyphenol compounds from all
fractions of the sugarcane juices.

Materials and Methods

HE ODS CARTRIDGE (S EP-P AK, V AC 35 CC , 10 G, C18 CAR -

tridge) was purchased from Waters Corp. (Milford, Mass.,

U.S.A.). An ultrafiltration unit (Model UHP150K) with a stirrer was purchased from Advantec Toyo Corp. (Tokyo, Japan). The ultrafiltration membrane was an Amicon YM100
membrane with molecular weight cut-off of 100,000 (Millipore Corp., Bedford, Mass., U.S.A.). Sugarcane extract (designated as MSX-1), containing polyphenols at high concentrations, was kindly provided by the Mitsui Sugar Co. Ltd.s
Development and Research Group, Chigasaki Laboratory
(Chigasaki, Japan). The Folin-Ciocalteu reagent was purchased from Nacalai Tesqu Corp. (Kyoto, Japan). The water
used was purified with a Millipore Elix 3. The other chemical
reagents and solvents were of analytical grade and used without further purification.
Commercially available sugarcane of the F160 variety
was obtained from a field in an Okinawa prefecture. Prior to
236

JOURNAL OF FOOD SCIENCEVol. 67, Nr. 1, 2002

use, the milled juice was frozen and stored at 20 C.

A solid phase extraction technique was used to recover
the polyphenols in the sugarcane. To determine the volume
of juice for ODS treatment, loading tests on the Sep-Pak cartridges were carried out by using MSX-1 Sugarcane Extract
as a model of the polyphenols in sugarcane. The ODS cartridge was activated, and a 0.1% MSX-1 Sugarcane Extract
aqueous solution was loaded onto the cartridge. Then, absorbance (OD340nm) of the elution (C O) was measured and
plotted (CO/CI) as a function of the elution volume. Here, C I
denotes OD340nm of the 0.1% MSX-1 solution.

ODS treatment
To remove insoluble impurities, the following treatments
were conducted: the frozen sugarcane juice was defrosted,
and centrifuged at 17000 x g for 15 min. The supernatant was
the centrifuged juice (CJ).
Ultrafiltration is effective for clarifying sugarcane juice
(Kishihara and others 1989; Kishihara and others 1993). CJ
was subjected to ultrafiltration and the ultrafiltered juice (UJ)
was then subjected to ODS treatment.
An ODS cartridge was conditioned with pure water before
use. The UJ (1000 ml) was loaded onto the ODS cartridge at a
flow rate of 8.3 ml/min. The eluate was designated Sugar
Fraction (SF). The cartridge was washed with 120 ml of pure
water. These washings (SWF) were combined with SF and the
mixture was concentrated to 57.5 brix in vacuo to obtain
syrup. The syrup was next subjected to a crystallization test.
The residue on the cartridge was eluted with 170 ml of 20%
or 50% ethanol, and the eluates (PF1 and PF2, respectively)
were concentrated to dryness. The cartridge was regenerated with 120 ml of pure water. A schematic diagram of the
process is presented in Figure 1. The operation was carried
out 50 times.

Crystallization of sucrose
The syrup was subjected to a crystallization test by using
an automatic laboratory boiling pan, as reported previously
by Kishihara and others 1994. The first obtained crystals
were called A-sugar. The mother liquid was called A-molasses. The crystallization was carried out 3 times and B-sugar,
C-sugar, B molasses, and C molasses were obtained, respectively (Table 1)

Analytical methods
Polyphenol was determined using Folin-Ciocalteu re 2002 Institute of Food Technologists

Decolorizing sugarcane juice

Results and Discussion

HE ADSORPTION CAPACITY OF ODS AND DESORPTION CON -

ditions were examined by using the commercial MSX-1

Sugarcane Extract as a model of polyphenols in sugarcane
juice. As a result of preliminary experiments, the concentration of polyphenols in sugarcane juice was found to be approximately 0.1%. From this, the concentration of MSX-1
Sugarcane Extract was adjusted to 0.1%, and the solution was
loaded onto the ODS cartridge. The OD340nm of the elution
(CO) was measured and the C O/CI ratio plotted as a function
of the elution volume (Figure 2). The CO/CI ratio was 0.1, 0.3,
0.66, and 0.91 after 1000, 2000, 3000, and 4000 ml elutions, respectively. It is preferred to obtain juice with as low a color
value as possible and to treat sugarcane juice in as large a
volume as possible. A 0.1 C O /CI ratio is equal to 90% decolorization. From these results, the treatment volume was determined as 1000 ml.
Stepwise elution was used, since sugarcane juice contains

Table 1Color values of the sugars and molasses

Color Value (IU)
A-sugar
B-sugar
C-sugar
Granulated sugar
Raw sugar

Color Value (IU)

48
99
342
< 10
3860

A-molasses
B-molasses
C-molasses

726
1510
3053

polyphenols of diverse polarity. The cane juice was clarified

according to the schematic diagram shown in Figure 1. The
operation described in Figure 1 was carried out 50 times to
evaluate the life span of the ODS cartridge. The color value
average for UJ and SF was 4226 and 376 IU, respectively. Decolorization (%) was maintained at about 90% after 50 repetitions (Figure 3). In another experiment performed in our
laboratory, ODS was compared with ion-exchange resin for
its ability to decolorize and for its life span using raw syrup.
The recovery of sucrose by crystallization is considered
an important index of juice clarification. The mineral content
of the juice is also an important index.
To evaluate the clarification, the syrup (concentrate of SF
and SWF) was subjected to a crystallization test. Photographs

Food Engineering and Physical Properties

agent, according to the method of Singleton and others

(1965). Gallic acid was used as a standard.
The color value was measured at OD420nm, and calculated according to the method of the International Commission
for Uniform Methods of Sugar Analysis (ICUMSA 1994). The
value was expressed as ICUMSA Units (IU). Decolorization
was calculated by the following equation:
Decolorization (%) = {( color value 0 - color value 1)/color
value 0} x 100
color value 0: color value before decolorization
color value 1: color value after decolorization
The potassium, calcium, and magnesium contents of sugar juice, before and after ODS treatment, were determined
by inductively coupled plasma spectrometry (Shimadzu
ICPS-1000 III) with sucrose solution as a matrix.

Figure 2Loading test of MSX-1 sugarcane extract of ODS

cartridge C o: OD340nm of outlet solution from the cartridge, CI: OD340nm of inlet solution to the cartridge

Figure 1Diagram of clarification of sugarcane juice

Figure 3Repetition loading test

Decolorizing sugarcane juice

Table 2Mineral contents before and after ODS treatment

Before ODS treatment (g/100g solid)

After ODS treatment (g/100g solid)

Ca

Mg

1.6
1.3

0.19
0.17

0.11
0.10

Table 3Total polyphenols and the recovery

Volume Concentration
Fraction (ml)
(%)
UJ
SF
SWF
PF1
PF2

Food Engineering and Physical Properties

of A-sugar, granulated sugar, and raw sugar are shown in Figure 4. A-sugar had a good shape and little color.
The mineral content of the juice before and after ODS
treatment is shown in Table 2. Most of the minerals were
found to remain after this treatment.
As mentioned above, ODS treatment did not remove minerals. It was therefore assessed that these minerals do not inhibit the crystallization of sugar. The color value of the sugars is shown in Table 2. The color value of A-sugar was below
50 IU (equivalent to most of the refined sugar available on
the market). To obtain refined sugar, 2 types of factories are
required, namely, a raw sugar factory and a sugar refinery. It
is possible for the refinery process to be omitted and obtain
white sugar.
Even for C-molasses, the color value was smaller than for
raw sugar. C-molasses from a sugar factory or refinery are
used in various kinds of fermentation as raw materials. However, the highly colored fermentation wastes can cause problems. The results of this study indicated that the ODS method, as described in this paper, can be used to eliminate this
waste problem.
After the juice was treated with ODS, the adsorbed
polyphenols were sequentially desorbed with 20 and 50%
ethanol solutions (Figure 1). The total concentration of the
polyphenols in each fraction was determined as mentioned
above and the results are shown in Table 3. The recoveries of
PF1 and PF2 were 28 and 7%, respectively. The main component of PF1 contains phenylpropanoids and their glucosides;
the main component of PF2 contains flavonoids and their Cglycosides (Yoshida and others 2000). These compounds exhibit strong antioxidant activity (Yoshida and others 2000).
The recovered polyphenols could be useful as antioxidants in
foods. Although more than 50% of the polyphenols moved to
the sugar fractions (SF and SWF), the remainder seemed to
have no negative effect on the color quality.
ODS treatment discharges little waste because ethanol is

1002
1010
122
170
167

Total
polyphenol
(mg)

*Polyphenol
recovery (%)

341
172
23
97
23

100
50
7
28
7

0.034
0.017
0.019
0.057
0.014

*Polyphenol recovery (%) was calculated based on the UJ

used for regenerating ODS. Thus it is possible to recover ethanol from PF1, PF2, and ethanol waste as described in Figure 1.

Conclusions

HE ODS TREATMENT PROPOSED IN THIS PAPER WAS VERY EF-

fective for clarification of sugarcane juice. A-sugar obtained from the juice had a pale color with 48 IU of color value. It may be possible to omit the refining step in the production of sugar. Even the color value of C-molasses
produced by this method was smaller than that of conventional raw sugar. Therefore, C-molasses could be used as a
raw material for fermentation without colored waste. The
polyphenols recovered from the ODS could conceivably be
used as an antioxidant in food. However, there are many
technical improvements needed before commercial practice.
Methods proposed in this study may realize a non-generated
waste, or green process, in the production of sugar.

References
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MS 20001596 Submitted 12/15/00, Revised 5/2/01, Accepted 5/24/01, Received
5/31/01
We express our deepest thanks to Chigasaki Laboratory, Mitsui Sugar Co. Ltd., for providing
MSX-1 Sugarcane Extract and to Dr. Y. D. Hang and Dr. G. S. Stoewsand for their helpful
advice and encouragement.

Figure 4Photograph of sugar crystals

Author Okuno is with the Graduate School Science and Technology, and
author Tamaki is with the Faculty of Agriculture at Kobe University, 1
Rokkodaicho, Nada-ku, Kobe 657-8501, Japan. Direct inquiries to author
Tamaki (E-mail: tamaki@kobe-u.ac.jp).