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Effect of ethanol-water solution on the crystallisation of short chain amylose

from potato starch

Article  in  Starch - Starke · December 2015

DOI: 10.1002/star.201500300

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Starch/Stärke 2016, 68, 683–690 DOI 10.1002/star.201500300 683

RESEARCH ARTICLE

Effect of ethanol–water solution on the crystallization of short

chain amylose from potato starch
Yanqi Liu 1,2, Huifang Xie 1 and Miaomiao Shi 1,2

1
School of Food and Biological Engineering, Zhengzhou University of Light Industry, Zhengzhou, P.R. China
2
Collaborative Innovation Center of Food Production and Safety, Henan Province, P.R. China

In this study, B-type microcrystalline (BM) starch was prepared by acid hydrolysis and Received: October 26, 2015
crystallization of native potato starch. Then, BM was used as the raw material to prepare A þ V Revised: December 9, 2015
type starch in ethanol–water solution. The effects of the amount of ethanol, the treatment Accepted: December 17, 2015
temperature, and the time on the structure of the precipitates were investigated. The optimal
conditions to form A þ V type starch are 22 mL ethanol at 50°C, for 120 min. The onset
temperature (To), the peak temperature (Tp), the conclusion temperature (Tc), and the
gelatinization enthalpy (4H) of native potato starch, acid hydrolyzed potato starch (AH), BM type
starch, and A þ V type starch were estimated by differential scanning calorimetry (DSC). It
indicates that the AH starch has a more ordered and stable structure, while the A þ V type starch
is more difficult to gelatinize. Fourier transform infrared spectroscopy (FT-IR) indicated that the
intensities of the main infrared absorption peaks of the A þ V type starch were significantly
higher than those of the native, AH and BM type starches, although the peak shapes were similar.
SEM photos showed that the A þ V type starch consisted of a flat structure with irregular edges
and small, well-dispersed spherical particles. This study clearly showed that the A þ V type starch
exhibited weak thermal stability owing to the characteristics of the granules.

Keywords:
Crystallinity / Potato starch / Short chain amylose

1 Introduction mixture of A-type and B-type starches. V-type crystal

Starch is the principal carbohydrate in cereal grains and is an
important source of nourishment in humans. Starches can
be categorized into A, B, C, and V-types according to their X-
ray diffraction patterns [1–3]. Cereal starches show the A-type
pattern, while tuber starches show the B-type pattern [4].
Some roots and seeds produce C-type starch, which is a
Correspondence: Dr. Miaomiao Shi, School of Food and Biological
Engineering, Zhengzhou University of Light Industry, Zhengzhou
450002, P.R. China.
E-mail: chengzi3090@126.com
Fax: þ86-371-86609631
Abbreviations: AH, acid hydrolyzed potato starch; BM, B-type
microcrystalline; DSC, differential scanning calorimetry; FT-IR,
fourier transform infrared spectroscopy; RC, relative crystallinity;
SEM, scanning electron microscopy; To, onset temperature; Tp,
peak temperature; Tc, conclusion temperature; XRD, x-ray
diffraction; 4H, gelatinization enthalpy
structures are rarely found in native starches [5].
Starch contains two main types of polysaccharides: amylose
and amylopectin. Amylose is a linear polymer consisting of
(1!4)-a-D-glucose units with a very small extent of a-(1!6)
linked branches, while amylopectin possesses a lot more a-
(1!6) branch points [6]. Amylose shows a unique feature that
enables it to form complexes with a variety of molecules.
Monoacyl lipids and emulsifiers, as well as smaller ligands
such as alcohols or flavor compounds, are able to induce the
formation of left-handed single helices in amylose to form the
V-amylose [1, 3, 7]. Short chain amylose with an average degree
polymer between 11 and 30 was obtained from native starch,
which was debranched by low temperature treatment and acid
catalysed hydrolysis. In an aqueous solution, the conforma-
tional change from a random string to a single spiral structure
can be achieved in the presence of ligands to form V-type
complexes [8].
Different V-type structures have been described and
characterized, which were obtained with iodine, dimethyl

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684 Y. Liu et al.
sulfoxide [9], potassium hydroxide [10], and potassium
bromide [11]. A previous investigation has also elucidated
the structure of the V-type amylose complexed with selected
flavor compounds such as menthone, fenchone, and
geraniol. Such complexes have been characterized by a
food model system [12–14]. Variations in the starch
crystalline structures arise from different molecular
arrangements and crystal orientations [15, 16]. Gao
et al. [17] have shown that the A-type structure of corn
starch change to the A þ V type after heat–moisture
treatment, while the B- and C-type structures present in
potato and pea starches change to the A-type.
However, little work has been reported on the relative
crystallinity, the physicochemical properties, and the granu-
lar structure of the A þ V type starch. Moreover, crystalliza-
tion of short chain amylose in the ethanol–water solution has
not been studied. Therefore, the effects of the amount of
ethanol, the treatment temperature, and the thermal
treatment time on the structures of the precipitates were
investigated. The differences in the properties of the native,
AH, BM, and A þ V type starches were also studied.
Therefore, this study provided a deeper understanding of
the A þ V type structure, which would help to figure out the
applications of modified starch in the food and non-food
industries.
2 Materials and methods
2.1 Materials
Native potato starch was purchased from Hengyang
Import & Export Co. Ltd., Henan, China. The native
potato starch has 25.3% amylose, 19.48% moisture,
0.36% ash, 0.10% protein, and a little fat. A LG10-24A
high speed centrifuge was supplied by the Beijing
Medical Centrifuge Co. Ltd., P.R. China. The electro-
thermostatic water bath was supplied by the Beijing
Yongguangming Medical Instrument Co. Ltd., P.R.
China. A Scientz-10N freeze dryer was supplied by the
Ningbo Xinzhi Biotechnology Co. Ltd., P.R. China. The
reagents used here were of analytical grade (HCL,
ethanol).
2.2 Preparation of AH
AH was prepared according to the method of Liu et al. [18]
with some modifications. Native potato starch (150 g) was
added to aqueous hydrochloric acid (500 mL, 2.2 mol/L) at
35°C. After 7 days, the suspension was washed several times
with deionized water until the pH was 7. After filtration, the
precipitate was washed with ethanol three times. Finally,
the solid was collected and dried in air to get the acid
modified starch for further applications.
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Starch/Stärke 2016, 68, 683–690
2.3 Preparation of BM
The above acid modified starch (5% w/w, 100 mL) was heated
in a boiling water bath to fully dissolve the starch. Then the
solution was cooled to room temperature and centrifuged to
remove insoluble substances. The supernatant was stored at
18°C for 12 h, then thawed slowly at room temperature.
When only a small amount of ice remained, the residue was
immediately filtered, washed with cold water, and air dried at
room temperature to give the BM [19].
2.4 Preparation of A þ V type starch
BM (1 g) was added to deionized water (20 mL) and heated at
165°C in a three-necked bottle equipped with a condensing
unit until the solution became transparent. Then, 22 mL of
ethanol was added dropwise into the hot starch solution. The
resulting solution was heated for 10 min and placed in a
water bath at 50°C for 120 min, then cooled to room
temperature. A þ V type starch was obtained from the
solution which was allowed to stand for 24 h to crystallize,
followed by centrifugation at 3000 r/min for 10 min, and
freeze drying for 12 h.
2.5 XRD analysis
Starch sample (0.5 g) was placed in a rectangular opening on
an aluminum plate (opening size: 15–20 mm; thickness:
1.5 mm) and pressed. XRD (BurkerD8, Germany) was used
to characterize the measurement of the starch samples, and
the wavelength of the monochromatic Cu–Ka rays used was
0.1542 nm. Other test conditions included a tube voltage of
3 kV, the pipe flow of 20 mA, the scanning speed of 4°/min, a
scan area of 5–35°, a sampling step width of 0.02°, and 1
repetition [20]. The calculation method devised by Komiya
and Nara was applied to process the crystallinity of the XRD
curve [21].
2.6 SEM analysis
Samples were mounted on metallic stubs, and then coated
with gold (50 s) with a sputter coater (Polaron Sputter Coat
System, Model 5001, England). The starch granules were
observed and photographed by SEM (Rili Co. Ltd., Japan).
2.7 DSC analysis
Perkin–Elmer DSC8000 (Norwalk, CT, USA) differential
scanning calorimeter (DSC), equipped with the thermal
analysis software Pyris window (Perkin–Elmer), was used to
measure and record the gelatinization temperature of the
starch samples. For this purpose, a solid sample suspension
with a weight ratio of 30% was prepared and stored in a
sealed DSC pan. Equilibration was performed at room
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Starch/Stärke 2016, 68, 683–690 Effect of ethanol–water solution. . . 685

temperature for 2 h. Then, the samples were heated from 30

to 150°C, at a heating rate of 10°C/min. To, Tp, Tc and DH
were calculated automatically [22].

2.8 FT-IR analysis

Starch sample (2 mg) and dry KBr (150 mg) were fully mixed
in a high speed mill, and put into the pressure medium
voltage to prepare tablets approximately 1 mm thick. Then,
the sample was analyzed in FT-IR (S3000, BIO-RAO,
America). Test conditions: the range of scanning wave
number was 4000  400 cm1 and resolution was 4 cm1.
The DTGS detector was used and air was used as blank. An
average of 32 scans provided the infrared spectrum of the
sample.

2.9 Statistical analysis

Duncan’s multiple range test (p < 0.05) was run by using

SPSS 17.0 Statistical Software Program (SPSS Incorporated,
Chicago) to analyze various (ANOVA) mean values. The data
in this report were analyzed and reported by using the Origin
Program 8.0 (Origin Lab Company, USA).

3 Results and discussion

3.1 Effect of the amount of ethanol on the starch

samples

Different concentrations of the starch samples were added to

ethanol–water solutions and boiled for 10 min. Then, the
solutions were cooled to 55°C and maintained for 120 min.
The XRD patterns of the samples are shown in Fig. 1a, with
crystallinity values shown in Table 1.
For the sample treated with 12 mL ethanol, the diffraction
patterns were mainly composed of four characteristic peaks
at 2u ¼ 15, 17, 18, and 23°. These are typical diffraction
patterns of the A-type starch. It is in agreement with the
conclusion by Liu et al. [23]. He reported that short chain
amylose tended to form an A-type structure, while long chain
amylose tended to form a B-type structure. The peaks of the
samples (treated by ethanol from 17 to 32 mL) at 13, 17, 20°
(2u) are the typical characteristics of a V-type structure. It can
be explained that ethanol induced the formation of left- Figure 1. X-ray diffraction patterns of different starch samples: (a)
handed amylose single helices to form the V-complex. It has the effect of the amount of ethanol, (b) the effect of treatment
temperature, and (c) the effect of treatment time.
been reported that many ligands can form inclusion
complexes with amylose. Their presence induces a confor-
mation change involving the transformation of amylose suggested that the A þ V type structure was produced in the
double helices into a single helix. The resulting so called ethanol–water solution. The results of Liu et al. [24] also
V-amylose is compact, and has a central hydrophobic cavity showed that a large number of ethanol can induce the starch
in which the hydrocarbon chain of the ligand can reside [8]. crystal to change from type B to type A þ V. From Table 1, the
Meanwhile, all the samples (treated by ethanol from 17 to RC of the V-type structure ranging from 0.00 to 10.64%
27 mL) exhibited the A þ V type diffraction pattern. This increases at first, then decreases. On the other hand, the RC

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686 Y. Liu et al. Starch/Stärke 2016, 68, 683–690

Table 1. Analysis of X-ray diffraction peaks crystallinity of process in which the crystal structure was formed through a
different ethanol amount of starch samples
hydrophobic interaction. Heat is conducive to the formation
Ethanol amount (mL) RC of V-type (%) RC of A-type (%) Total RC (%) of a crystal structure. Higher temperature also enhances the
activities of the starch and ethanol molecules to form a more
12 0.00 43.84 43.84 crystalline structure [8, 23]. The formation of a complex may
17 4.08 36.00 40.08 be inhibited by gelatinized amylose, with a disrupted helical
22 10.64 29.07 39.71 structure caused by high temperature. It can, therefore, be
27 8.82 33.78 40.82 concluded that 50 °C was conducive to the formation of the
32 6.91 33.92 42.60
V-type crystalline structure for the starch samples.

3.3 Effect of the thermal treatment time on the starch

of the A-type structure (from 33.70 to 43.80%) showed an
opposite trend compared to the V-type structure with an
increase in the amount of ethanol. However, the total RC of
the samples changed slightly. The results are in agreement
with the previous report that suggested that most of the
amylose which has the ability to crystallize will produce a
crystalline structure. The mixed solvent system can partly
change the single helical structure into a double helix in
solution, so that different crystalline conformations are
produced [19].
3.2 Effect of the treatment temperature on starch
samples
The starch samples were added to 22 mL of ethanol and
boiled for 10 min. Then, the solution was cooled to different
treatment temperatures, and maintained for 60 min. The
XRD patterns of the starch samples are shown in Fig. 1b. All
the samples exhibited an A þ V type diffraction pattern. It
suggested that the products were the mixtures of the A- and
V-type structures. It is probably because the starch tends to
produce a B-type structure at lower temperatures (5°C) and
an A-type structure at higher temperatures (35°C) [23].
The differences in the crystallinity (Table 2) between
starch samples are attributed to the differences in the
amount of crystalline regions, which is influenced by the
amylose content and the amylopectin CLD [25]. The RC of
the V-type structure ranging from 5.09 to 12.46% increases at
first, then decreases with increased temperature. The results
can be explained by considering that it is an endothermic
samples
The starch samples were added to 22 mL of ethanol and
boiled for 10 min. Then, the solution was cooled to 55 °C, and
maintained at that temperature for different time periods.
The XRD patterns of the starch samples are shown in Fig. 1c.
All the samples showed the typical A þ V type X-ray
diffraction pattern with a fairly strong intensity for the
corresponding peaks. The intensity of all the peaks changed
slightly over time. It suggested that no significant differences
occurred in the X-ray diffraction patterns among the starch
samples over time.
The crystallinity values are listed in Table 3. For the
sample treated for 120 min, the RC of the V-type structure
reached a maximum of 12.00%, while that of the A-type
structure reached a minimum of 26.91%. The total
crystallinity changed slightly from 36.28 to 45.09%. It can,
therefore, be concluded that thermal treatment time has little
effect on complex formation.
3.4 Granular structure of starches
The shape and surface characteristics of the native and
treated starches are shown in Fig. 2. Native starch granules
were kidney-shaped, spherical, or oval, with varied sizes. The
smaller starch granules were spherical and the larger starch
granules were oval, but the kidney shape was common for all
granule sizes [26]. Acid hydrolysis did not alter the shape and
the integrity of the starch granules. The BM-type starch
showed a relatively uniform spherical particle size, with
adhesion between crystal particles. Melting on the surface of
the area of crystallization had led to fusion between the

Table 2. Analysis of X-ray diffraction peaks crystallinity of

different thermal treatment temperature of starch
samples Table 3. Analysis of X-ray diffraction peaks crystallinity of
different thermal treatment time of starch samples
Treatment temperature (°C) RC of V-type (%) RC of A-type (%) Total RC (%)
Treatment time (min) RC of V-type (%) RC of A-type (%) Total RC (%)
40 5.09 34.54 39.63
45 11.76 23.15 34.91 60 9.93 35.16 45.09
50 12.46 22.04 34.50 90 6.90 35.06 41.96
55 12.13 25.97 40.62 120 12.00 26.91 38.91
60 9.05 31.57 38.10 150 7.67 28.61 36.28

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Starch/Stärke 2016, 68, 683–690
crystal particles [19]. In general, the shape of the A-type
microcrystalline starch was spherical, and it commonly
exhibited the phenomenon of material deposition on the
surface. This was due to the deposition of the starch chains in
solution on the surface of the crystals during the crystal
growth process at room temperature, which occurred after
the basic formation of the crystals. The deposition
phenomenon was also partly related to incomplete crystalli-
zation on the surface, which could also result in deformation
during the process of drying [18]. The A þ V type starch
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Effect of ethanol–water solution. . . 687
Figure 2. SEM of (A) native potato starch, (B) AH
starch, (C) BM starch, and (D) A þ V type starch.
consisted of a flat structure with irregular edges and small
spherical particles. The shape of the particles in the V-type
structure was obvious and mostly flat. There was hardly any
adhesion between the crystal particles that were well
dispersed.
3.5 Thermal properties of starches
The thermal parameters of native, AH, BM, and A þ V type
starches, determined by DSC, are summarized in Table 4.
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688 Y. Liu et al.
Table 4. Thermal parameters of native, AH, BM, and A þ V type starches
Samples To (°C) Tp (°C)
Native starch 69.46  0.02d 75.30  0.00c
AH starch 68.85  0.02c 82.39  0.01d
BM 62.66  0.02b 73.67  0.02b
A þV type starch 53.88  0.01a 69.00  0.01a
Values with different letters in the same column are significantly different (p < 0.05).
a) PHI (peak high index) ¼ 4H/(Tc–To).
Native potato starch had an endothermic transition ranging
from 69.46 to 84.19°C, with enthalpy of 16.58 J/g. To
decreased slightly from native starch to A þ V type starch.
Tp provided a measure of the crystallite quality [27]. The
higher Tp value in the AH starch suggested that it had a more
ordered and stable structure that required a higher melting
temperature [28]. The value of (Tc–To) can be interpreted as a
measure of the homogeneity of the crystalline and the
noncrystalline conformations, whereas 4H reflected the
extent of order, i.e., the enthalpy of melting the crystals and
the double helices [29]. The values of (Tc–To) reflected the
degree of difficulty in gelatinizing the starch granules. The
higher the value of (Tc–To), the more difficult it was for
the starch to be gelatinized, and vice versa. The values of
(Tc–To) for the A þ V type starch reached a maximum, which
suggested that it was difficult to gelatinize the starch.
However, the enthalpy of the A þ V type starch reached a
minimum. This indicated that there was a small proportion
of defective crystallites in the A þ V type starch that resulted
in it the lowest gelatinization temperature and enthalpy. This
could be due to the degradation of some amylose chains that
were involved in the formation of double helical structures
with either amylose or amylopectin chains [30]. The peak
high index (PHI ¼ 4H/(Tc–To)) has been used to measure
the uniformity in gelatinization by researchers [31]. It can be
seen in Table 4 that the PHI of all the three treated starches
were lower compared to that of the native starch and that of
the A þ V type starch was far lower than the others. A lower
uniformity in the gelatinization of the A þ V type starch
could also be found.
3.6 FT-IR analysis
Fourier transform infrared spectroscopy is an important
method to analyze and detect the composition and
structure of samples. Infrared spectroscopy can also be
used to determine whether ligands complexed with starch
and to determine the structural differences between
samples. The material composition, conformation, con-
figuration, and crystalline structure of the starch samples
were studied. The results of the native potato starch, the
AH starch, the BM starch, and the A þ V type starch are
shown in Fig. 3.
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Starch/Stärke 2016, 68, 683–690
Tc (°C) Tc–To 4H (J/g) PHIa)
84.19  0.01b 14.73 16.58 0.12b 1.1
104.64  0.22d 35.79 17.16  0.46c 0.5
83.03  0.01a 20.37 20.96  0.09d 1.0
92.11  0.03c 38.23 3.82  0.03a 0.1
The location of the major infrared absorption peaks of
the four samples changed slightly. The intensity of the
major infrared absorption peaks of the A þ V type starch
was significantly higher than that of the native AH and BM
starch samples. Nevertheless, the peak shapes were similar.
The peak near 1600 cm1 could be attributed to the
vibration frequency of the aldehyde group in starch. The
absorption peaks of 1000 cm1 to approximately 1300 cm1
can be attributed to the stretching vibration frequencies of
the C–O–C bond. The absorption peak for BM starch could
be seen at 3427.2 cm1, which could be the vibration
frequency for the –OH group in glucose residues. The peak
of the A þ V type starch shifted to a lower wave number at
3394.3 cm –1 due to the association and superposition of the
–OH groups in starch and ethanol. The absorption peaks
near 2900 cm1 are the characteristic peaks for the
methylene group. Both the A þ V type and BM starch
samples showed peaks at 2927.9 cm1. The peak intensity
of the former was stronger than that of the latter due to a
superposition with the methylene groups of ethanol. With
ethanol as the ligand, the intensity and sharpness of the
absorption peaks at 1012.6 and 1364.3 cm1 of the A þ V
type starch increased, which can be attributed to the –OH
group in the compounds, their crystalline structure, and the
nature of the ligand.
Figure 3. FT-IR patterns of (a) native potato starch, (b) AH starch,
(c) BM starch, and (d) A þ V type starch.
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Starch/Stärke 2016, 68, 683–690
4 Concluding remarks
In the present study, starch with the A þ V type crystalline
structure could be produced from the BM-type starch and
ethanol under certain experimental conditions. The RC of
the V-type structure increased at first, then decreased with
the amount of ethanol. It showed the same trend with
increasing temperature. Thermal treatment time had little
effect on complex formation. The optimal conditions for the
formation of the A þ V type structure were the use of 22 mL
ethanol at 50°C, for 120 min.
Starch with A þ V type crystalline structure was charac-
terized by granules, with a flat structure and small spherical
particles. It was more difficult to gelatinize this starch
compared to the native starch, the AH starch, and the BM
starch. However, AH starch has a more ordered and stable
structure. These results are important for exploring the use
of potato starch with special advantages and contribute to
understanding the potential characteristics of the modified
starch in traditional Chinese crop.
We are grateful to the National Natural Science Foundation
of China (no. 21376228).
The authors have declared no conflicts of interest.
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