Journal of Food Engineering 77 (2006) 295303

www.elsevier.com/locate/jfoodeng

Gelation properties of axseed gum

Hai-Hua Chen, Shi-Ying Xu *, Zhang Wang
School of Food Science and Technology, Southern Yangtze University, Wuxi, Jiangsu 214036, PR China
The Key Lab of Food Science and Safety, Ministry of Education, 214036, PR China
Accepted 6 June 2005
Available online 11 August 2005

Abstract
The gel formation and the eects of dierent factors on the gel strength of axseed gum gel were studied. The results showed that
axseed gum could form thermoreversible cold-setting gel. Both gelling and melting points increased with increment in dissolution
temperature. While at the same dissolution temperature, the gelling point was lower than its corresponding melting point. Because
the gel strength dropped down with decreasing pH values at pH 26 or increasing pH values above pH 9, the maximum gel strength
was obtained at pH 69. The addition of Na+ lowered the Zeta potential, thus decreasing the gel strength. But the eect of divalent
cation Ca2+ on the gel strength was in two ways. Low concentration of CaCl2 (<0.3%, w/w) increased the gel strength because of
facilitating the formation of three-dimensional networks by Ca2+ cross-linking; but high concentration of CaCl2 (>0.3%, w/w) had a
negative eect by decreasing Zeta potential. Adding axseed gum to carrageenan gel decreased the syneresis of gel.
 2005 Elsevier Ltd. All rights reserved.
Keywords: Flaxseed gum; Gelling temperature; Melting temperature; Gel strength; Microstructure

1. Introduction
Flax (Linum usitatissimum L.) is one of the oldest
crops known to man (Oomah, 1993), mainly for the
use of its oil and bre. The whole seed and oil of ax
have been used for edible purposes in some European
and Asian countries (Wanasundara & Shahidi, 1997).
Flaxseed gum comprises about 8% of the seed weight
(BeMiller, 1993); however, its yield is dependent on
extraction regimes (Cui, Mazza, & Biliaderis, 1994;
Fedeniuk & Biliaderis, 1994; Mazza & Biliaderis,
1989). Because axseed gum is commercially feasible
only as a by-product of the linseed oil industry, preparation methods of gum are based on oil meal or oil meal
cake (BeMiller, 1993). Flaxseed gum is a heterogeneous
polysaccharide composed of xylose, arabinose, glucose,
galactose, galacturonic acid, rhamnose and fucose

Corresponding author. Tel./fax: +86 510 5884496.

E-mail address: syxu@sytu.edu.cn (S.-Y. Xu).

0260-8774/$ - see front matter  2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2005.06.033

(Chen, Xu, & Wang, 2004a; Cui et al., 1994; Erskine

& Jones, 1957; Hunt & Jones, 1962; Muralikrishna, Salimath, & Tharanathan, 1987). Flaxseed gum is a hydrocolloid with good water-holding capacities, owing to its
marked swelling capacity and high viscosity in aqueous
solution (Chen, Xu, & Wang, 2004b; Fedeniuk & Biliaderis, 1994). Functionally, axseed gum resembles
gum arabic more closely than the other common gums,
so that it has been suggested to replace gum arabic in
emulsions (BeMiller, 1993; Mazza & Biliaderis, 1989).
Flaxseed gum also exhibits weak gel-like properties
that can be used to replace most of the non-gelling gums
for food and non-food applications (Chen et al., 2004b;
Cui et al., 1994; Yoshihara Oil Mill Ltd., 1981). Gel
forming biopolymers can be divided into cold-setting
and heat-setting, based on the two main gelation
mechanisms: gelation induced by cooling or by heating,
respectively (Doublier, Launay, & Cuvelier, 1992; Silva
& Rao, 1999). Gel systems can be divided into two classes: true gels and weak gels, depending upon the
macroscopic behavior. A weak gel exhibit ow

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H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

properties when submitted to high enough stress, in

which, there is a higher dependence on frequency for
the dynamic moduli, suggesting the existence of relaxation processes even at a short time scale, and a less difference between moduli values indicating the lower
percentage recovery of the stored energy. The macromolecule substances to form network structure in food
systems are primarily polysaccharides and proteins.
Carrageenan is an anionic sulphated polysaccharide
extracted from red algae, mainly composed of D-galactans and 3, 6-anhydride galactans. There are three types
of carrageenan including j-, k- and i-types. The j-carrageenan with KCl can form a kind of sti and brittle gel
which is easy to syneresis (Glicksman, 1983; Therkelsen,
1993). In general, addition of a few gums such as locust
bean gum and konjac glucomannan to carrageenan can
lower syneresis.
There has been increased interest recently in the physical and functional properties of axseed gum (Cui &
Mazza, 1996; Cui, Kenaschuk, & Mazza, 1996;
Fedeniuk & Biliaderis, 1994; Mazza & Biliaderis, 1989;
Wannerberger, Nylander, & Nyman, 1991). However,
the weak gel-like properties of axseed gum have
not been studied in detail. The aim of the present work
was to study the gel formation, the eects of dierent
factors on the gel strength and microstructure of axseed gum extracted from China-Sinkiang-cultivated axseed using thermal analysis, rheology measurement, gel
strength measurement, Zeta potential measurement,
atomic force microscopy as well as scanning electron
microscopy. The eect of axseed gum on syneresis of
carrageenan was also studied by rheology measurement.

2. Materials and methods

2.1. Materials
Sample of axseed gum was provided by Sinkiang
Luqi Biotechnology Ltd. (Sinkiang Province, China).
j-Carrageenan was provided by Hainan Duohuan
Healthy Food Ltd. (Shanghai, China).

12 by adding 0.1 mol/l HCl or 0.1 mol/l NaOH. For

samples containing salts, the concentration of NaCl or
CaCl2 or complex phosphate salts (mixture of sodium
tripolyphosphate, sodium metaphosphate and sodium
pyrophosphate) in gels varied from 0.1% to 2%.
For Zeta potential analysis, 0.08% solutions of axseed gum were prepared.
Flaxseed gum and carrageenan were mixed at various
ratios which contained 0.1% KCl. The total polysaccharide concentration was xed at 1% (w/w).
2.3. Dynamic measurements
Dynamic rheological experiments were performed
using an AR1000 Rheometer (TA Instrument Ltd., England). The linear viscoelastic region was determined for
each sample through stress sweeps at 1 Hz. Viscoelastic
properties (storage modulus G 0 and loss modulus G00 ,
tan d) of axseed gum solutions were determined within
the linear viscoelastic region (Mohamed & Xu, 2003).
The data reported is the average of at least two
replicates.
During gelling and melting temperature experiments,
a cone-and-plate geometry with a diameter of 60 mm
and a cone angle of 1 was used. A cover, treated with
liquid paran, was applied to prevent evaporation (Baeza, Carp, Perez, & Pilosof, 2002). The samples were
heated from 10 C to 60, 70, 80 and 90 C at a rate of
8 C/min and held for 2 min. The samples were then
cooled to 10 C at 5 C/min and kept at 10 C for
10 min to ensure a homogenous gel system. Finally,
the samples were reheated to 90 C at a rate of 5 C/
min. The temperature at which G 0 and G00 crossed was
taken as the gelling point during cooling. The melting
point was also evaluated at the point where G 0 and G00
crossed during reheating.
Viscoelastic properties of axseed gum/carrageenan
mixtures were determined using the AR1000 Rheometer, using parallel plate geometry (diameter 40 mm,
gap size 1.5 mm). A cover, treated with liquid paran,
was applied to prevent evaporation. The mechanical
spectra were made using temperature sweeps from 10
to 90 C at 10 C/min at a constant frequency of 1 Hz.

2.2. Preparation of samples

2.4. DSC measurements
For gelling and melting temperature measurements,
1% (w/w) solutions of axseed gum were prepared by
stirring with magnetic stirrer at room temperature to
make axseed gum swelling fully.
For gel strength measurements, 2% (w/w) axseed
gum solutions were prepared at certain temperature.
The gels were then formed by cooling and keeping at
48 C overnight before gel strength measurements.
For samples prepared at dierent temperatures, the temperature varied from 60 to 95 C. For samples prepared
with dierent pH, pH value was adjusted from pH 2 to

A Pyris-1 DSC calorimeter (PE Ltd., USA) was used

to obtain thermal transition temperatures.
About 20 mg of the sample was sealed into the DSC
pan hermetically. An empty sealed pan was used as reference (Eleya & Turgeon, 2000). The sample pan and
reference pan were then placed inside the calorimeter
and heated from 10 C to 60, 70, 80 and 90 C at
8 C/min, respectively, and kept for 2 min to ensure that
the solution was homogenous. The temperature was
then lowered to 10 C at a rate of 5 C/min, kept for

H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

10 min, and raised again at the same rate up to 90 C.

Finally, the enthalpy proles were recorded. The data
reported is the average of at least two replicates. The
peak temperatures of exothermic peak and endothermic
peak were described as gelling point and melting point,
respectively.
2.5. Longitudinal compression measurement
Longitudinal compression measurements were
performed on TA XT2i Texture Analyser (SMS Ltd.,
England). The gels were packaged in cylindrical containers of 60 mm in diameter and 80 mm in height. The gels
were subjected to compression tests using a cylindrical
probe (0.5 in. in diameter). The probe was lowered at
a speed of 2.0 mm/s and compressed to 50% of their original height. The average of at least ve replicates was
reported. The maximum force making the gel rupture
was described as gel strength.
2.6. Zeta potential measurement
The Zeta potential was measured at 20 C on a Malvern Zetasizer 2000 (Malvern Instrument Ltd., England)
across the capillary tube. Before measurement, samples
were ltered through 0.45 lm lter. The average of three
replicates was reported.
2.7. Gel syneresis
Gel syneresis, revealing the water-holding ability, was
measured as the percentage of supernatant liquid after
centrifugation of the gel at 8000g (4 C) using a GL20B freezing centrifuge (Shanghai Anting Instruments,
China) for 20 min.
2.8. Atomic force microscope (AFM)
For imaging, axseed gum powder was dispersed in
distilled water to make a concentration of 1 mg/ml, stirred overnight, diluted to 10, 25, and 50 lg/ml, respectively, then heated at 95 C with stirring for 20 min.
Aliquots (2 ll) of the diluted sample solutions were
immediately spread onto freshly cleaved mica surfaces
and imaged in the tapping mode with an etched silicon
tip Nanoprobe attached to 125 lm long cantilever, with
a resonant frequency in the range 200400 kHz and a
spring constant of 2080 N/m by AFM (Nanoscope
IIIa, Digital Instrument, CA). Topographical images
were obtained at constant amplitude and recorded
simultaneously with the complementary amplitude
mode data. The image analysis was carried out using
the Nanoscope III software (Version 5.12r2, Digital
Instruments, Veeco).

297

2.9. Scanning electron microscope (SEM)

Flaxseed gum gels were xed in 1% (w/w) osmium
tetroxide solution for 16 days at 4 C. The xed samples
were rinsed in phosphate buer (pH 7.2, 0.1 M) over 10
times and then dehydrated through a graded series of
alcohol concentrations (30%, 50%, 70%, 90% and
100%). The samples were then immersed in isoamyl acetate and dried in a critical point drier (model CPD-030,
BAL-TEC company). The specimens were coated with a
thick by use of an ionic
layer of gold/palladium, 200 A
sputter (model SCD-005, BAL-TEC company) and observed in the scanning electron microscope (model
QUANTA-200, FEI company, accelerated voltage was
operated at 10 kV).

3. Results and discussion

3.1. Gelling and melting temperature of axseed gum
The variations of storage modulus (G 0 ) and loss modulus (G00 ) with temperature during gelling and melting
processes were shown in Fig. 1 for 1% solutions of axseed gum. In the rst heating process from 10 to 60 C,
axseed gum exhibited weak gel-like properties when
temperature lower than 40 C, i.e., G 0 > G00 (see
Fig. 1A). Both G 0 and G00 were strongly temperature
dependent. When cooling (see Fig. 1B), G 0 and G00 both
increased with decreasing temperature. And at around
45 C they showed a cross-over (gelling temperature)
when initial cooling was done from 60 C, which indicated that gelation had developed. When reheating
(see Fig. 1C), G 0 and G00 both decreased with increasing
temperature, and crossed again (melting temperature) at
47 C, which suggested that melting had occurred. These
results implied that axseed gum solutions could form
cold-set gels. Fig. 2 showed DSC curves for axseed
gum solutions during gelling and melting process. The
cooling curves (A) had a distinct single exothermic peak,
while the reheating curves (B) had an endothermic peak,
indicating gelling occurred during cooling process and
melting during heating process. Both rheology and
DSC measurements showed that the axseed gum gel
was a thermoreversible gel, which melted when heating
and gelled when cooling.
Gelling temperature (Tgel) and melting temperature
(Tmelt) of axseed gum solution were shown in Table 1.
Both Tgel and Tmelt were strongly dependent on the
initial cooling temperature. Higher initial cooling temperature meant higher dissolution temperature. Gel
point depended on dissolution temperature, i.e., gels
formed at higher temperatures. The reason was that at
higher dissolution temperature, molecules exhibited
much larger hydrodynamic radius due to sucient
hydration and extension (Bemiller & Whistler, 1996;

20

15

1.5

10

0.5
G'

tan

G''

0
5

(A)

25
45
Temperature ( C)

65

20

Fig. 2. DSC curves for 1% (/w/w) axseed gum solution during gelling
and melting (initial cooling temperature is 60 C): (A) cooling process
and (B) reheating process.

1.5

15
1
10

40

0.5

5
G'
5

(B)

G''

Gel strength (g)

G ' o r G " (P a )

25

tan

H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

tan

G ' o r G " (P a )

298

tan
0

25
45
Temperature ( C)

65

35

30
20
10

21
1
14

70

G'

G''

25

(C)

45
Temperature ( C)

90

100

strength. Thus, more energy was needed to break the ordered network resulting in higher melting temperature.
Tgel was lower than the corresponding Tmelt at the same
initial cooling temperature as shown in Table 1. Because
the gelling process and melting process of food hydrocolloids were followed by DG = DH  T DS, gelling process
being a spontaneously exothermic process. So, lowering
temperature facilitated the gelling process. On the contrary, melting process belonged to an unspontaneously
endothermic process (He, 2001). Thermal motion energy
could not overcome the interaction force which formed
networks if the temperature was only increased to Tgel.
Extra energy was needed to complete the breakage of
the ordered network on the account of higher Tmelt than
the corresponding Tgel (Baeza et al., 2002; He, 2001).

tan
0

80
Temperature (C)

Fig. 3. Eect of dissolution temperature on gel strength of axseed

gum.

0.5

7
0

60

1.5
tan

G ' o r G " (P a )

0
28

65

Fig. 1. Temperature dependence of storage modulus, loss modulus

and tan d for 1% (w/w) axseed gum solution during gelling and
melting processes (initial cooling temperature is 60 C): (A) rst
heating process; (B) cooling process and (C) reheating process.

Chen, Xu, & Wang, 2004c; He, 2001). Flaxseed gum

molecules formed three-dimensional network easily at
higher temperature during cooling. Junction zone numbers also increased with higher initial cooling temperature, which caused denser network and higher gel

Table 1
Gelling and melting temperature (Tgel and Tmelt) for 1% (w/w) axseed gum solution
Method

Tgel or Tmelt (C)

60

70

80

90

Rheology

Tgel
Tmelt

45.1 (0.1)
47.0 (0.1)

52.2 (0.5)
58.5 (0.2)

61.3 (0.9)
67.1 (1.2)

66.6 (0.2)
79.3 (1.1)

DSC

Tgel
Tmelt

40.8 (0.02)
43.1 (0.05)

46.9 (0.1)
49.5 (0.04)

52.8 (0.15)
55.6 (0.1)

55.0 (0.05)
67.3 (0.1)

Initial cooling temperature (C)

H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

The values of rheology measurement and DSC measurement were not absolutely equal as shown in Table
1. This was attributed to dierent measurement principles. DSC measurement reected energy changes during
gelling-to-melting transition (Nishinari, 1997), but rheology measurement reected viscoelasticity changes
(Doublier et al., 1992).

299

3.2. Gel strength of axseed gum

3.2.1. Eect of the dissolution temperature
Dissolution temperature had a large eect on the gel
strength. As shown in Fig. 3, raising dissolution temperature increased the gel strength of 2% (w/w) axseed gum. This might be associated with an increased

Fig. 4. Atomic force microscopy images of axseed gum deposited onto mica: (A) 25 C, 24 h, 25 ll/mg, 1 lm 1 lm; (B) 60 C, 20 min, 25 ll/mg,
1 lm 1 lm; (C) 95 C, 20 min, 10 ll/mg, 1 lm 1 lm; (D) 95 C, 20 min, 25 ll/mg, 1 lm 1 lm and (E) 95 C, 20 min, 50 ll/mg, 2 lm 2 lm.

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H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

hydrodynamic radius because of sucient hydration

and extension of axseed gum molecules, stronger
molecular interaction and more junction zones caused
in higher dissolution temperature. This was also veried
by the AFM images as shown in Fig. 4A, B and D.
Fig. 4A showed that axseed gum solution could not
form a gel network dissolved at lower temperature.
Fig. 4D showed that axseed gum solution formed a
denser gel network dissolved at higher temperature,
which could oer more resistance to the applied force
resulting in gel rupture.
3.2.2. Eect of concentration
The gel strength and microstructure of axseed gum
depended on concentration of axseed gum. The results
in Fig. 5 showed that the gel strength was concentration
dependent. The gel microstructures in Fig. 4CE illustrated that higher concentration increased molecular
numbers and strengthened molecular interactions,
which resulted in formations of more junction zones.
3.2.3. Eect of pH value
The pH values had dierent eects on the gel strength
of axseed gum at acidic or alkaline conditions (Fig. 6).
Based on decreasing gel strength in the range of pH 26
and above pH 9, the maximum gel strength was obtained at pH 69 and varied relatively insignicantly.

Flaxseed gum is an anionic polysaccharide which

bears a negative charge due to ionized carboxyl group
(Chen et al., 2004a; Cui et al., 1994). Intermolecular
electrostatic repulsion due to homo-charges makes the
molecular chains fully extended and interpenetrated
with each other, to form intermolecular cross-linking
which induced gelation. Since net electrostatic repulsion
decreased at low pH value, the interaction of molecules
also decreased, leading to reduction in gel strength. At
higher pH values, the decrease in gel strength might be
attributed to alkaline depolymerization reaction, resulting in less junction zones (BeMiller, 1993; Fedeniuk &
Biliaderis, 1994).
3.2.4. Eect of salts
The responses in gel strength of axseed gum with
addition of dierent valence mineral salts are shown in
Fig. 7. Dierent salts had dierent eects on the gel
strength. Initial addition of NaCl resulted in reduction
of the gel strength, which attributed to compression of
the double electric layer of molecules. While addition
of CaCl2 up to 0.3% resulted in increase of gel strength
and the converse was obtained above 0.3%. As the Zeta
potential was lowered (Fig. 8), the intramolecular charge
repulsions decreased progressively. The polysaccharide
molecules were contracted and the junction zone numbers were decreased due to the addition of monovalent
and divalent cations (Mazza & Biliaderis, 1989). Flaxseed gum possesses 14% galacturonic acid which attaches to the backbone of molecular chain (Chen

120

G e l s tre n g th (g)

Gel strength (g)

40
90
60
30
0

3
2
Concentration (%,w/w)

30
20
10

5
0

Fig. 5. Eect of concentration of axseed gum on the gel strength.

0.5

1
Concentration (%, w/w)

1.5

0.5

1
Concentration (%, w/w)

1.5

(A)
50
G e l s tr e n g th (g)

Gel strength (g)

40
30
20

40
30
20
10

10

0
0

pH
Fig. 6. Eect of pH values on the gel strength of axseed gum.

(B)

Fig. 7. Eect of dierent valent mineral salts on the gel strength of

axseed gum: (A) NaCl and (B) CaCl2.

H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

0
Z e ta p o te n tia l (m V )

Zeta potential (mV)

0
-10
NaCl

-20

CaCl2
-30
-40

301

-10
-20
-30
-40

0.5

1
Concentration (%, w/w)

1.5

Fig. 8. Eect of dierent valent mineral salts on the Zeta potential.

0.5

1
Concentration (%,w/w)

1.5

Fig. 10. Eect of complex phosphate salts on the Zeta potential.

et al., 2004a; Hunt & Jones, 1962). Ca2+-induced crosslinking between axseed gum molecules promoted to
form three-dimensional networks when adding small
amounts of CaCl2 to the gels, as commonly observed
for pectin (Bemiller & Whistler, 1996). But the shielding
eect of electrostatic repulsion was predominant when
adding large amounts of CaCl2. Thus, the formation
of three-dimensional networks was inhibited and gel
strength decreased correspondingly.
3.2.5. Eect of complex phosphate salts
Complex phosphate salts (mainly Na+ salts) are additives used in meat processing. Flaxseed gum can also be
used in the meat products (Dev & Quensel, 1989). The
eects of complex phosphate salts on gel strength are
studied and the results were shown in Fig. 9. The addition of complex phosphate salts resulted in reduction of
the gel strength, ascribed to the decrease of the Zeta potential (Fig. 10) and contraction of the polysaccharide
molecules.
3.3. Gel microstructure
SEM provided microstructure information about the
gel. The micrographs in Fig. 11 showed the three-dimensional networks of axseed gum gel. From Fig. 11B, it
can be seen that the gel network was getting denser with
increasing of concentration of axseed gum solution.

Gel strength (g)

40
Fig. 11. Microstructure of axseed gum gel determined by SEM: (A)
0.5% and (B) 1.0%.

30
20

3.4. Eect of axseed gum on syneresis of carrageenan

10
0

0.5

1
Concentration (%,w/w)

1.5

Fig. 9. Eect of complex phosphate salts on the gel strength.

The eects of the addition of axseed gum into carrageenan on the gel strength, syneresis and viscoelastic
properties were presented in Figs. 12 and 13. When
the total polysaccharide concentration was xed at 1%
(w/w), the gel strength of mixed gels gradually dropped

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H.-H. Chen et al. / Journal of Food Engineering 77 (2006) 295303

800

20
syneresis

600

15

400

10

200

0.1
0.2
0.3
0.4
Addition of flaxseed gum (%, w/w)

Syneresis (%)

Gel strength (g)

gel strength

0
0.5

Fig. 12. Eect of addition of axseed gum on the syneresis and gel
strength of axseed gum/carrageenan blends (total polysaccharide
xed at 1%).

1.2

0.9
1
0.6

ta n

G ' o r G '' ( P a )

10

0.1
0.3
G'
0.01
0

G''

tan

0.05
0.1
0.15
Addition of flaxseed gum (%)

0
0.2

Fig. 13. Eect of addition of axseed gum on tan d, G 0 and G00 of

axseed gum/carrageenan blends (total polysaccharides xed at 1%).

and syneresis signicantly decreased with the addition of

axseed gum. If the concentration of axseed gum was
0.08%, the syneresis of the axseed gum/carrageenan
gel decreased from 11.01% (free of axseed gum) to
6.63%. Syneresis reduced nearly 40% and the gel
strength lowered only 10%. The storage modulus G 0 reects the solid-like properties, loss modulus G00 reects
the liquid-like properties, while tan d(G00 /G 0 ) reects the
proportion of viscosity to elasticity in the system. When
G 0 decreased gradually, whereas G00 and tan d increased
with the addition of axseed gum, the viscosity
increased with the addition of axseed gum. The
water-holding capacities increasing with the viscosity
increment could explain why the mixed gel syneresis
dropped with addition of axseed gum.

4. Conclusion
Flaxseed gum solutions were characterized with gelation that could form a thermoreversible cold-set gel. The
gelling and the melting points of axseed gum were
inuenced by the initial cooling temperature, and the
gelling temperature was lower than its corresponding
melting temperature. The dissolution temperature, pH

value, addition of dierential valence mineral salts affected the gel strength of axseed gum. Raising dissolution temperature increased the gel strength. The
addition of NaCl and complex phosphate salt decreased
the gel strength. The addition of CaCl2 had an unusual
eect on the gel strength. Low concentration of CaCl2
(<0.3%, w/w) increased the gel strength, but high concentration of CaCl2 (>0.3%, w/w) decreased the gel
strength. Adding axseed gum to carrageenan gel increased the viscous and decreased the syneresis.
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