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RESEARCH ARTICLE
1
College of Food and Bioengineering, Qilu University of Technology, Jinan, Shandong, P.R. China
2
Shandong Provincial Key Laboratory of Fine Chemicals, Jinan, Shandong, P.R. China
3
Shandong Institute of Metrology, Jinan, Shandong, P.R. China
The micro-structural changes of jams containing different amounts of cross-linked acetylated Received: November 5, 2013
starch (CAS) have been studied using rheological measurements, sensory evaluation, scanning Revised: February 23, 2014
electron microscopy (SEM), and laser particle analysis. The results indicated that all samples Accepted: February 27, 2014
exhibited pseudoplastic ow with yield stress. Subsequent dynamic oscillatory rheological study
also showed that jam structure was more compact in the presence of 20% CAS. SEM analysis
demonstrated that there was a ne, homogeneous network in the microstructure of apple jams.
Furthermore, it was found that the particle size was smaller after adding CAS. Therefore, we
conclude that CAS could be an appropriate gelling agent for apple jams, and the most suitable
CAS content for industrial manufacturing was 20%.
Keywords:
Jam / Microstructure / Particle size / Rheological behavior / Sensory evaluation
the results from Matignon et al. [13] suggested that they can apple pulp was weighed using an electronic scale (0.1 mg),
even slightly penetrate into the starch granules. which was then treated with a 10% w/v citric acid solution to
Sensory evaluation, a statistical approach using human afford the mixture with a desire pH (pH 3.5), followed by
senses, is based on taste, color, odor, spreadability, and overall adding certain amount of sugar and CAS. Specically, apple
acceptability of consumer products. Notably, a consumer often pulp (100 g), sugar (15 g) and CAS (0, 15 g, 20 g, or 25 g) were
judges the product quality (freshness, staleness, tenderness, combined and the resulting mixture was stirred continuously
and ripeness) when the food in his mouth produces a physical with a glass-rod at the boiling temperature. Heat was removed
sensation (hard, soft, crisp, moist, or dry) [1416]. The when TSS reached 65Brix or above. The obtained mixture
ascending forced choice test for taste and smell is a widely was subsequently milled with a colloid mill to afford a
used method, in which samples are often evaluated by uniform product, which was poured into a 200 mL glass
increasing the intensity to a given point. Particularly, the beaker and sealed while hot. Finally, the sample was sterilized
combination of sensory analysis and mechanical measure- at 100C for 20 min and then cooled down to 40C.
ments, such as the textural and rheological analyses, can
determine the jam quality more precisely. 2.3 Rheological measurements
The rheological behavior of jams has been extensively
studied in the literature [1721], and it appears that they are The rheological properties of apple jams were measured
mainly affected by the following factors: the amount and type using a rheometer (BOHLIN C-VOR150, Malvern, United
of sugar added, acidity, proportion and kind of pectin used, Kingdom) with 40 mm parallel-plate geometry at 25C. For
fruit pulp content, and process temperature. However, less apple jam samples, the steady ow measurements were
attention has been paid to the microstructure of jam products. carried out within the range of shear stresses corresponding
Recently, the microstructure of mango jams has been studied, to the shear rates from 1 to 100 per second. The duration of
using SEM analysis, and the results indicate that such jam is measurements was 503.9 s. All experiments were conducted
composed of network regions with large pores and dense, in triplicate, at least. The steady-state relationship between
compact regions with small pores [21]. At present, studies to shear stress and shear rate of food material can be described
extend the application of cross-linked acetylated starch (CAS) with a HerschelBulkley model [22].
to apple jams are still scarce in the literature.
t t0 Kg n 1
In this work, the rheological properties of apple jams
containing different amounts of CAS have been investigated, where t is the shear stress (Pa), t0 is the yield stress (Pa), is
and their structural characteristics, particle size, and spatial the shear rate (s1), K is the consistency index (Pa sn), and n is
distribution were also examined. In addition, we sought to the ow behavior index which represents the extent of
understand the effect of CAS on the rheological, textural, and deviation from Newtonian behavior.
micro-structural characteristics of apple jams, which can be Stress sweep tests (test range: 1100 Pa) were performed
employed to study the feasibility of replacing pectin with CAS to determine the linear viscoelastic region of all samples at a
in jam manufacturing. frequency of 1 Hz. Frequency sweep tests were conducted
from 100 to 0.01 Hz at a stress yield of 10 Pa. The elastic
modulus (G0 ), the viscous modulus (G00 ), and the loss tangent
2 Materials and methods angle (tan d), as a function of frequency, were obtained by
calculating with Bohlin software (Version 6.20).
2.1 Materials
2.4 Sensory evaluation
The cross-linked acetylated cassava starch (CAS) with a
1.935% degree of substitution (DS) was prepared in the Taste, color, odor, spreadability, and overall acceptability of
Shandong Provincial Key Laboratory of Fine Chemicals. Citric apple jam samples were evaluated using the nine point
acid was supplied by Henan Quartz Food Additive Company. hedonic scale (9 like extremely, 8 like very much, 7 like
Apples and sugar were purchased from the local market. moderately, 6 like slightly, 5 neither like nor dislike,
4 dislike slightly, 3 dislike moderately, 2 dislike very
2.2 Jam preparation much, 1 dislike extremely) [23]. Total 20 panelists partici-
pated in this study, and the scores were averaged to afford
Apple jams were prepared with starch and sugar at pH 3.5. mean values for further analysis.
The total soluble solid (TSS) (1Brix) was measured using a
hand refractometer (WAZ-1, Shanghai, China). A PB-10 pH 2.5 Microstructure
meter (Sartorius, Germany) was employed to measure the pH
of jams. The TSS and pH of the apple pulp used in jam The morphology and microstructure of jam samples were
preparation was 14Brix and 4.4, respectively. At rst, 100 g of examined using SEM (QUANTA 200, Holland) and CLSM
Based on the relationship between shear stress and shear 3.2 Dynamic oscillatory test
rate, we evaluated the rheological properties of jam samples,
and the results are shown in Fig. 1 (25C). Notably, we found Important information about gel structure can be obtained
that the shear stress rose with the increase of shear rate, and from G0 and G00 , which often change with frequency.
all systems exhibited pseudoplastic ow with yield stress. In Specically, G0 is the dynamic elastic or storage modulus,
addition, shear thinning was clearly evident, as indicated by related to the material response as solid; G00 is the viscous
the fact that n was less than 1. The relationship between shear dynamic or loss modulus, related to the material response as
stress and shear rate can be described with the Herschel uid [32]. Figure 2 shows the values of G0 and G00 , and it
Bulkley model. The value of R2 in this study ranged from turned out that G0 was larger than G00 in most samples,
0.891 to 0.998, similar to the results obtained in strawberry exhibiting typical gel-like behavior [33, 34]. In addition, these
and apricot jams [26]. All samples exhibited yield stress and results also indicated that such samples were viscoelastic
their apparent viscosity decreased with the increase of shear uids. Even though G0 and G00 steadily increased with the
rate (these results were not shown here). As illustrated in frequency within a specic range (0.01 Hz<f<57 Hz), they
Fig. 1, the values of shear stress increased when the CAS varied erratically when the frequency exceeds 57 Hz, possibly
concentration was increased from 15 to 25%, presumably due due to the fact that the turbulence appeared during the
to the thickening effect of CAS. The value of yield stress is shearing process could substantially damage the apple jam
highly dependent on the quantitative and qualitative addition system. Consequently, the rheological properties of jam
Theoretically, tan d is closely related to the overall viscoelastic positive effect to the overall sensory quality of soups. Hence,
response, and a smaller value generally indicates a more we conclude that CAS can be employed as a gelling agent in
elastic sample [32, 42]. We found that the sample network apple jams, and 20% should be the most suitable CAS content
has gained more structure after adding CAS, especially for for the industrial manufacturing process.
sample 3, which is consistent with the trend of dynamic
curve. 3.4 Microstructure of apple jam samples
According to the data shown in Fig. 3b, complex viscosity
was also frequency dependent. All apple jam gels exhibited SEM was employed to investigate the micro-morphology of
shear-dependent ow behavior, while their complex dynamic the apple jam system, and the results are shown in Fig. 4.
viscosity linearly decreased with the increase of frequency. Sample 1 (without CAS) possessed a smooth surface, as
These results suggested that molecular interactions could illustrated in Fig. 4a. When CAS was gradually added into the
lead to the formation of gel structure at low frequency, but system, a ne homogeneous network was established, as
gave rise to fragmented structure at high frequency [34, 43]. shown in Fig. 4bd. These results clearly indicated that the
Apparently, compared with other CAS-containing samples, combination of CAS with one or a few substances (e.g.,
sample 3 exhibited the highest h , suggesting that it should pectin) in the original system could generate new reticulation.
possess the best viscoelasticity. Furthermore, the apple jam system containing certain
amounts of CAS should possess denser structure with small
3.3 Sensory properties of apple jams pores, especially in sample 3, which is in agreement with the
results obtained from the rheological analysis. In a word,
Sensory evaluation is one of the most important methods to the CAS added has made great contribution to the formation
examine the food preference of a consumer. In this work, the of network structure, which certainly would alter the micro-
sensory analysis was performed with 20 panelists. Apple jams texture and increase the water-retention of apple jams.
prepared with different concentrations of CAS were evaluated Moreover, confocal laser scanning microscopy (CLSM)
for color, taste, odor, spreadability, and overall acceptability. analysis was performed to characterize the continuous and
Sensory scores are summarized in Table 1. Notably, we found dispersed phases of jam samples. CAS was stained with a
that jams containing different amounts of CAS exhibited uorescent dye, Rhodamine B, which can be adsorbed
signicant differences in terms of taste, spreadability, and onto the starch granules, due to its afnity [11]. As shown in
overall acceptability. The scores of taste, spreadability, and Fig. 5, uorescence can be visualized on the periphery of
overall acceptability were improved by adding CAS to apple the swollen CAS granules, which is consistent with the
jams. Especially, the scores of overall acceptability for previous reports [11, 46]. Possibly, swelling CAS granules can
the apple jam with 20% CAS were the highest (p<0.05). have open pores on their surface, which would allow certain
These data showed that the sensory quality of jams was substances in the apple jam system (e.g., pectin) to permeate
closely related to its physical and rheological properties. The into the interior of granules. Consequently, a network
addition of CAS has improved the sensory quality of jams, structure would be formed due to the interaction between
presumably because it can lead to smaller particle size. This pectin molecules and CAS molecules.
result is in agreement with the report that the greater the
proportion of large particles comprising the sauce, the 3.5 Sample granule size
coarser its texture [44]. The highest score for overall
acceptability was obtained from the sample with 20% CAS, The granule size of sample 1, sample 2, sample 3, and sample
exhibiting a high storage modulus (G0 ) and loss modulus 4 was 148.991 3.356, 38.826 0.932, 42.559 1.135, and
(G00 ). Wongsagonsup [45] found that good rheological 40.236 0.967 mm, respectively. The particle size of sample 1
properties, i.e., strong gel structure, high shear resistance (without CAS) was close to the one reported by Mohr [47],
of the 1.0%-CLTS (cross-linked tapioca starch) could bring in which they have found that the intermediate size groups
1 6.85 0.81a 7.40 0.60b 6.70 0.58a 6.75 0.64a 6.10 0.55a
2 7.25 0.72a 7.05 0.69ab 7.85 0.67b 7.80 0.62c 7.20 0.41c
3 7.30 0.73a 6.85 0.75a 8.25 0.64c 8.40 0.50d 8.35 0.49d
4 6.80 0.77a 6.80 0.70a 7.65 0.59b 7.25 0.64b 6.55 0.61b
ad
Different letters within a column indicate signicant difference (p<0.05). Sample 1: apple jam without CAS; Sample 2: apple jam containing
15% CAS; Sample 3: apple jam containing 20% CAS; Sample 4: apple jam containing 25% CAS.
were 0.161.0 mm in apple sauce. The particle size of apple with modied starch. On the other hand, it appeared that the
jams prepared with CAS was dramatically decreased, concentration of CAS did not have signicant inuence on
presumably due to the fact that these systems contained the granule size of samples.
swollen modied starch granules. It was found that the One of the most noticeable characteristics for apple jams
particle size of starch granules is around 40 mm [44], which is containing CAS was the smaller particle size. Generally, a
consistent with our results. Juszczak et al. [48] also reported sauce containing higher proportion of large particles tends to
that the particle size of starch granules is 50 mm in ketchup afford coarser texture [44]. To our delight, the apple jam
prepared with CAS turned out to be a ne-textured product,
as illustrated by SEM analysis.
4 Conclusions
sensory evaluation experiments. Meanwhile, we found that [13] Matignon, A., Moulin, G., Barey, P., Desprairies, M. et al.,
the CAS-containing apple jams possessed more condensed Starch/carrageenan/milk proteins interactions studied using
multiple staining and Confocal Laser Scanning Microscopy.
and homogeneous network in their microstructure. More- Carbohydr. Polym. 2014, 99, 345355.
over, the addition of CAS also led to smaller particle size,
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and 20% CAS was the most suitable percentage for jam Food Sci. 1963, 28, 385389.
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