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Abstract: Health and wellness aspirations of U.S. consumers continue to drive the demand for lower fat from inherently
beneficial foods such as yogurt. Removing fat from yogurt negatively affects the gel strength, texture, syneresis, and
storage of yogurt. Amylosepotassium oleate inclusion complexes (AIC) were used to replace skim milk solids to improve
the quality of nonfat yogurt. The effect of AIC on fermentation of yogurt mix and strength of yogurt gel was studied and
compared to full-fat samples. Texture, storage modulus, and syneresis of yogurt were observed over 4 weeks of storage at
4 C. Yogurt mixes having the skim milk solids partially replaced by AIC fermented at a similar rate as yogurt samples
with no milk solids replaced and full-fat milk. Initial viscosity was higher for yogurt mixes with AIC. The presence of
3% AIC strengthened the yogurt gel as indicated by texture and rheology measurements. Yogurt samples with 3% AIC
maintained the gel strength during storage and resulted in low syneresis after storage for 4 wk.
Keywords: amylosefatty acid complex, rheology, storage, syneresis, texture, yogurt
Introduction
In the presence of hydrophobic ligands such as fatty acids, amylose undergoes conformational changes to form amylosefatty acid
inclusion complexes. The formation of amylosefatty acids inclusion complexes has been extensively studied and recently reviewed
in depth (Putseys and others 2010; Obiro and others 2012). Studies of these types of amylose complexes have dealt mostly with
their effect on the pasting properties of starch granules, structure
of the complexes, thermodynamic properties (Ghiasi and others
1982; Evans 1986; Biliaderis and Tonogai 1991; Eliasson 1994;
Svensson and others 1998; Gelders and others 2006; Mira and
others 2007a, b), and their ability to retard retrogradation of starch
in baked products (Keetels and others 1996). Amyloselipid complexes have been proposed and examined as a means of delivering
ligands with desired functional properties in food products. One
important use is to deliver unsaturated fatty acids, nutraceuticals
(Cohen and others 2008), and volatile flavor (Heinemann and others 2005; Wulff and others 2005; Conde-Petit and others 2006;
Itthisoponkul and others 2007) or aroma (Jouquand and others
2006; Tietz and others 2008) compounds while protecting them
from oxidation.
Recently, we have been examining the preparation and properties of starch materials containing amylosesodium palmitate inclusion complexes obtained by blending jet-cooked high-amylose
corn starch with aqueous solutions of sodium palmitate (Fanta and
others 2010; Byars and others 2012). At appropriate fatty acid salt
concentrations to effectively complex the amylose, a low-viscosity
dispersion results that displays no evidence of starch retrogradation upon standing for extended periods. These dispersions exhibit polyelectrolytic characteristics, and at high pH, electrostatic
repulsion between the anionic carboxylate head groups of the
MS 20131368 Submitted 9/26/2013, Accepted 12/30/2013. Authors are with
USDA, Agricultural Research Services, Natl. Center for Agricultural Utilization Research, 1815 N. Univ. St., Peoria, IL, 61604, USA. Direct inquiries to author Singh
(E-mail: mukti.singh@ars.usda.gov).
complexed fatty acid salt stabilizes the amylose polymer in solution and inhibits intermolecular interactions between the amylose
molecules. As the pH of the dispersion is lowered, the carboxylate
anion is protonated and converted into its corresponding fatty acid
that reduces the electrostatic repulsion of the amylose complex.
When this occurs, physical associations form between the amylose
molecules generating a stable 3-dimensional gel network (Byars
and others 2012).
Fat plays a significant role in gel strength, texture, and syneresis of yogurt. Stabilizers in low-fat yogurts are used to strengthen
the 3-dimensional network structure formed by casein micelles
at low pH. Various nondairy ingredients such as starch, whey
protein concentrates, gelatin, and hydrocolloids have been added
to yogurt as fat replacers and to modify the rheological properties (Mistry and Hassan 1992; Keogh and OKennedy 1998;
Guzman-Gonzalez and others 1999; Decourcelle and others 2004;
Sodini and others 2004). The addition of whey protein concentrates can lead to powdery taste, excessive acid development, excessive firmness, higher syneresis, and grainy texture (Mistry and
Hassan 1992; Guzman-Gonzalez and others 1999). Addition of
starch increases the viscosity of yogurt, but some starches impart
an undesirable taste and promote phase separation. Addition of
inulin improved the texture of no fat yogurt but increased yogurt
syneresis (Pimentel and others 2011). In our previous studies, we
found that starchlipid composites strengthened low-fat set-style
yogurts (Singh and Byars 2009; Singh and Kim 2009).
The objective of this study was to examine the suitability of
amylosefatty acid salt complexes as stabilizers in nonfat yogurt.
We chose potassium oleate instead of sodium palmitate as used in
our previous studies for nutritional superiority. These complexed
starches can be simply prepared on large scale using commercially
available steam jet cookers and renewable low-cost commodity
amylose-containing starches and fatty acid salts.
E822
R
C 2014 Institute of Food Technologists
doi: 10.1111/1750-3841.12378
Further reproduction without permission is prohibited
calculated from weight loss after drying at 100 C under vacuum, and all starch weights are given on a dry weight basis.
Oleic acid, 99%, was purchased from Nu-Check Prep (Elysian,
Minn.). Ethanol (95%) was purchased from Decon Laboratories, Inc. (King of Prussia, Pa., U.S.A.). Potassium hydroxide,
>85%, pellets/certified ACS, was purchased from Fisher Chemical
(Pittsburgh, Pa., U.S.A.).
The general procedure of de Mul and coworkers was used for
the preparation of potassium oleate (de Mul and others 2000).
A solution of oleic acid (33.53 g, 0.118 mol) in 95% ethanol
(130 mL) was prepared by stirring and warming to 50 C. To
the solution, 51 mL of 2.53 M KOH in 95% ethanol was slowly
added while stirring. After addition, the solution was stirred an
additional 30 min at 50 C and then removed from the heat and
cooled to room temperature (approximately 22 C). The solution
was further cooled to 4 C and allowed to crystallize undisturbed
overnight. The resulting crystals were vacuum filtered in a Buchner
funnel, washed with cold 95% ethanol, and vacuum-dried in
a desiccator. The yield of potassium oleate obtained was 65.1%
(24.5 g).
tan (Pa)
(16.5 h)
Yogurt mix
viscosity Pas
82
418
232
382
605
0.18
0.21
0.18
0.16
0.15
0.0019
0.0024
0.11
0.41
0.3
Skim control
Full-fat control
1% AIC
2% AIC
3% AIC
(2009) found that mix viscosity in itself did not affect the final gel
structure of yogurt.
Onset time of gelation was defined as the time when the storage
modulus exceeded 3 Pa. Fat content in yogurt mix significantly
affected onset time of gelation (Figure 2). Full-fat milk yogurt
mix had significantly lower onset time of gelation compared to
skim milk yogurt mix. Removal of fat in yogurt mix delayed the
gelation process during fermentation. Xu and others (2008) also
reported low-fat samples needed more incubation time for commencement of gelation in comparison to full-fat milk. Addition
of AIC induced earlier gelation relative to skim milk control yogurt, and at 3% AIC gel began to form almost as early as for
full-fat milk control yogurt. This indicates that AIC can replace
fat without affecting the gelation of yogurt.
Effect of AIC on formation of the yogurt gel at 40 C is shown
in Figure 3. The storage modulus, G , was measured at a frequency
of 1 rad/s to monitor gel strength during fermentation. A long
induction time was observed for each sample, during which the
modulus value was below the measurement threshold. The storage
modulus increased rapidly for each sample as gel began to form,
and then continued to increase throughout the fermentation. The
level of starch complex affected both the time at which gel growth
was first observed and final value of storage modulus. The initial
growth rate of the storage modulus was similar for each sample,
but yogurts containing starch complex continued to increase in gel
7.0
skim control
1%
2%
3%
full fat control
6.5
240
6.0
180
Time [min]
pH
Yogurt texture
Texture of yogurts set in 4 oz bottles was measured using
TA XT2i Texture Analyzer (Texture Technologies Corporation,
Scarsdale, N.Y., U.S.A.). Yogurt samples were evaluated in triplicates using stainless steel ball probe (TA 18) set for a 10 cycle
test. The test parameters were 5 mm/s test speed, 2 mm/s pretest
speed, 5 mm/s posttest speed, 10 g trigger force, and a distance of
10 mm. All measurements were recorded as the force (g) of the
peaks. The maximum force for the 1st peak (g) was used to determine firmness, whereas ratio of the maximum force of the tenth
peak to the maximum force of the 1st peak was used to evaluate
gel resiliency. All tests were conducted in duplicates at ambient
temperature with product temperature near 4 C. Samples were
taken directly from refrigerator and placed on instrument stage for
the measurements.
5.5
5.0
skim control
full fat control
AIC
60
4.5
4.0
120
60
120
180
240
300
Time [min]
360
AIC [%]
103
102
skim control
full fat control
1%
2%
3%
creased for samples with starch complexes (Table 1). A lower value
of loss tangent indicates a firmer gel, so a firmer yogurt gel was
formed with starch complexes compared to either skim milk or
full-fat milk yogurts.
Storage modulus, G measured at a frequency of 1 rad/s for all
yogurts samples during storage at 4 C, is presented in Figure 5.
All yogurt samples maintained gel strength during storage of 4 wk.
Yogurt samples with fat (full-fat control) had significantly higher
storage modulus in comparison to skim milk yogurt control. The
storage modulus increased with increasing AIC concentration in
skim milk yogurt stored for 4 wk.
Color of yogurt
Total color of yogurt samples is presented in Figure 6. Full-fat
yogurt samples had higher total color values that were attributed
to higher lightness (L ). Addition of AIC to skim milk resulted
in reduced total color attributed to lower lightness in yogurt.
However, the difference in total color among yogurts was not
obvious to naked eye.
G' [Pa]
Texture of yogurt
Initial firmness of yogurt, as 1st peak force measured by texture analyzer during storage, is shown in Figure 7. As expected,
101
full-fat milk yogurt was significantly firmer than skim milk yogurt during 29 d of storage, suggesting a positive interaction of
fat globules with the casein gel network in yogurt. Martin-Diana
and others (2004), Pereira and others (2006), Aziznia and others
100
(2008), and Yazici and Akgun (2004) also observed that fat significantly increased gel firmness. Addition of 3% AIC to skim milk
yogurt mix significantly increased firmness of the yogurt. This is
in agreement to the observations from rheology data described
10-1
above. This confirms our assumption that AIC plays the role of fat
0
60
120
180
240
300
during yogurt fermentation.
Final firmness at the end of cycle as the 10th peak force of all
Time [min]
yogurt samples followed a similar trend as initial firmness, but was
Figure 3Effect of level of amylosepotassium oleate complexes in skim significantly lower.
milk on the onset time of gelation during yogurt fermentation. Onset time
is defined as G > 3 Pa.
104
6000
skim control
full fat control
1%
2%
3%
5000
4000
[Pa]
103
102
skim control
full fat control
1%
2%
3%
101
10-2
10-1
100
[rad/s]
101
3000
2000
1000
0
102
15
22
29
Time [day]
Figure 4Linear viscoelastic spectra after 16.5 h of storage at 4 C. The Figure 5Effect of storage time at 4 C on linear viscoelastic spectra
storage modulus G is shown with solid symbols and the loss modulus G is (storage modulus G ) for full-fat milk yogurt and yogurt various amylose
potassium oleate complex levels (0%, 1%, 2%, and 3%) in skim milk.
shown with open symbols.
Vol. 79, Nr. 5, 2014 r Journal of Food Science E825
strength faster than the full-fat control yogurt. At the end of 330
min fermentation period, 3% AIC yogurt mix formed stronger
gel than full-fat control (Table 1).
Storage and loss (G ) moduli are shown for all samples in
Figure 4 after holding in the rheometer at 4 C for 16.5 h. Results
for each sample are characteristic of a gel, with G > G at all
frequencies, and with both values showing very little frequency
dependence. Values here are higher than those in Figure 3 primarily due to lower measurement temperature, but full-fat control
showed a greater increase upon cooling and had the highest modulus values at 4 C. Frequency dependence of the moduli does
not suggest any qualitative differences in the yogurts formed with
starch complexes. However, the loss tangent (tan = G /G ) de-
100
100
80
Resiliency [%]
90
80
skim control
full fat control
AIC
70
60
40
20
0
60
skim control
full fat control
1%
2%
3%
15
22
29
Time [day]
AIC [%]
100
30
skim control
full fat control
1%
2%
3%
25
20
60
Syneresis [%]
Firmness [g]
80
40
20
0
skim control
1%
2%
3%
full fat control
15
10
5
15
22
Time [day]
29
15
Time [day]
22
29
Figure 7Effect of storage on the firmness of yogurts made full-fat milk and Figure 9Effect of storage on syneresis of yogurts made full-fat milk and
various amylosepotassium oleate complex levels (0%, 1%, 2%, and 3%) various amylosepotassium oleate complex levels (0%, 1%, 2%, and 3%)
in skim milk.
in skim milk.
Conclusion
Yogurt mixes with skim milk solids replaced by amylose
potassium oleate complexes (AIC) or milk fat, fermented lactose to lactic acid at a rate similar to those with no milk solids
replaced. Positive interaction of AIC (3%) with yogurt network
strengthened skim milk yogurt gels, reduced syneresis, and behaved similar to full-fat yogurts. Yogurts with 3% AIC maintained
strong gel structure during 4 wk of storage at 4 C. AIC provides an alternative method to strengthen low-fat yogurts. This
study demonstrates that AIC can be added to replace fat in yogurt
mix, without affecting structural characteristics and storability of
set yogurt. However, further study is needed to understand the
mechanism of interaction by which AIC induces earlier onset of
gelation with increased gel strength, without affecting the fermentation of lactose to lactic acid in yogurts.
Acknowledgment
Technical assistance provided by AJ Thomas and Wilma Rinsch
during the course of this study is gratefully acknowledged.
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