study on gelatinization property and edible quality mechanism of rice

RESEARCH ARTICLE

Study on gelatinization property and edible qualitymechanism of rice

Ting Huang1*, Bo Zhu1*, Xuezhu Du2, Bin Li1,3, Xiaofang Wu1 and Shishuai Wang1

1 College of Food Science and Technology, Huazhong Agricultural University, Wuhan, P. R. China2 College of Life Science, Hubei University, Wuhan, P. R. China3 Key Laboratory of Environment Correlative Dietology (Huazhong Agricultural University), Ministry of Education, P. R. China

The different quality of rice in simulated cooking process was investigated by using SEM,

FT-IR, XRD, and DSC methods. The result shows that the starch granules of rice of low

amylose content (AC) have more pores and cavities, which directly led to the swelling of rice

starch granule. With the change in temperature, the changes in intensity and width of the IR

bands showed that the variation in proportion area of crystalline to non-crystalline was related

to AC of rice. According to the interpretative sensitivity of the data obtained, XRD method

was suggested adequate for characterizing the pasting property of different quality of rice.

Besides, DSC method showed the AC was not relevant to pasting temperature and enthalpy.

Received: November 22, 2011

Revised: April 16, 2012

Accepted: April 24, 2012

Keywords:

Amylose / Edible quality mechanism / Gelatinization property / Rice

1 Introduction

Starch is widely used in food industry. Gelatinization and

gelation of starch are considered as basic processes in the

making of starch containing foods. A range of consecutive

changes involved in starch gelatinization and gelation play

a key role in processes such as bread baking, gelling of pie

fillings, etc. The conditions in which the phenomena com-

prised in these processes, determine the quality of the final

food products [1, 2].

Starch degradation does not occur uniformly. SEM can

be used to examine the granules produced after amylosis.

Starch occupies a high proportion of the world’s food-

energy intake. Before consumption, starchy food materials

are generally heated to a state, leading to a transition,

which is known as gelatinization. Thus, gelatinization is an

important operation in food preparation and processing.

The transition entails a loss of structural order for example,

the starch double helices disappear, though some of the

resultant polysaccharide coils may form a different helical

structure by interacting with lipids.

A long-established trend in food research is to take the

principles underlying the methods of studying synthetic

polymers, and to apply these to food systems.

In the gelatinization process, water molecules are

absorbed by the amorphous region when diffusing into

the starch granule, then combined with the starch granules

in the radial expansion of water, which lead to the optical

birefringence and crystal ordering disappearing. Finally,

AM leaching and the double helix structure of crystalline

regions gradually expand and dissociate. SEM is mainly

used for observing surface morphology, granule size of

starch, and analyzing the structural variations of starch

granules [3].

The IR spectrum of starch has been proven to be

sensitive to changes in structure on a molecular level

(short-range order), such as starch chain conformation,

helicity, crystallinity, and retrogradation processes, as well

as water content [4]. Infrared was used in the past to study

AM, amylopectin, and starch to provide information on

*These authors contributed equally to this work as co-firstauthors.Additional Correspondence: Xuezhu DuE-mail: [email protected]

Correspondence: Professor Bin Li, College of Food Science andTechnology, Huazhong Agricultural University, Wuhan, 430070,P. R. ChinaE-mail: [email protected]: þ86-27-87282966

Abbreviations: AC, AM content; HRD, hardness; RT, roomtemperature; SR, swelling ratio; WAR, water absorption ration

DOI 10.1002/star.201100177Starch/Starke 2012, 00, 1–9 1

� 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.starch-journal.com

chain folding and the ratio of ordered to amorphous frac-

tions. The sensitivity of infrared to the order within starch

samples has been subject to debate. However, infrared has

been shown sensitive to short-range order in numerous

publications. It can produce a significant impact on

physical and chemical characteristics of samples [5].

Van Soest et al. [6] found that the IR A band at 1047/cm

was sensitive to the amount of ordered or crystalline

starch, and the band at 1022/cm is a characteristic of

amorphous starch. Consequently, the ratios of the bands

at 1047–1022/cm expresses the crystallinity of starch

granules in the short range [6].

Natural starch granules are mainly two types of X-ray

characteristics diffraction pattern as follow. The first is

known as the typical A-type, including cereals like rice,

maize, and wheat starch; the second is the B-type, which

is based on tubers such as potatoes and bananas starch.

XRD method is used to measure the length sequence that is

the order of molecules formed by starch molecule chains.

Unlike the previous description of FT-IR, X-ray character-

istics diffraction was widely used as the most direct way of

estimating the degree of crystallinity, crystal size [7].

On the other hand, correlation between infrared and

XRD is obtained for mixtures of crystalline and amorphous

starch. XRD reports long-range order such as the packing

of double helices into ordered arrays.

Starch is biosynthesized as semi-crystalline granules

with varying polymorphic types and degrees of crystallinity

[8]. During gelatinization, the ordered crystals turn into

the disordered non-crystalline ones with an energy

change [9]. Different reactive thermodynamic properties

and energy between starch and water change because of

the tightness of granules, the ratio of AM and AP, and

branches densities of AP vary from different sources

of the starch, [9]. DSC can detect the thermodynamic

properties so as to provide support for thermodynamics

investigation of starch.

In recent advances in the study of cereal-based food

systems, thermal events such as melting and glass transition,

have been of much interest to food scientists in both

industrial field and academic circles. The structural com-

ponents, responsible for these products (mostly starch),

play a key role in determining the desired textural quality, for

example, crunchiness, softness/moistness, hardness (HRD),

etc. In addition, deterioration of texture is a common subject

of study in terms of molecular mechanisms, with the aim of

minimizing or inhibiting the deterioration. Thus, character-

ization of cereal biopolymers by thermal analysis is an

important approach to the understanding of the function-

ality of starch on both structural and molecular level.

Previous theoretical work on predictive models relating

physicochemical properties to texture of cooked rice and

the application of rice blends shows that AM content (AC)

has a significant correlation with textural properties and the

principal component factor analysis results indicates that

AC is the first factor [10]. Therefore, different pasting

properties of various AC rice starch in cooking process

are studied to elucidate mechanism of its edible quality.

Therefore, the objective of this study was attempting to

compare starch gelatinization of different quality of rice

and its links with eating quality by SEM, FT-IR, XRD, and

DSC method.

2 Materials and methods

2.1 Materials

Rice samples are Enuo9 (Amylose11.6), Guangliangyou-

558 (Amylose24.00) and Yangliangyou419 (Amylose28.00).

2.2 Scanning electron microscopy (SEM)analysis

Rice flour was affixed to the loading platform by using a

double-sided adhesive tape, then the treated platform was

put into a surface processor. After spraying gold, the plat-

form was removed. The surface morphology of starch

granules was observed in 0.1 t vacuum by scanning elec-

tron microscope (JSM-6390), with the magnification of

500� and 4000�. The working conditions of SEM are:

High-voltage 20 kV, beam 5 � 10�9 mA, working distance

15 mm [11, 12].

2.3 Variable temperature Fourier transformsinfrared spectroscopy (FT-IR) analysis

Rice flour and water (1:1.2) were mixed into a starch milk,

then the KBr slide was covered with the starch milk before it

was placed into the variable temperature slot of Nicolet

6700 FTIR at bath temperature (RT-1008C). Then scan-

ning was operated at different infrared temperature points,

with the spectral scanning range being 4000–400/cm,

distinguishability being 4/cm and number of scanning

times being 32. Meanwhile, temperature was kept for

10 min for each temperature point [13].

2.4 X-ray diffraction (XRD) analysis

D/MAX-RB type X-ray diffractometer was used to measure

the crystallinity of rice power, which is treated under differ-

ent temperature, with a Cu Ka target at 40 kV and 50 mA.

The diffraction angle ranging from 55 to 58, scanning

speed being 108C/min and step being 0.02.

The crystallinity of the starch was calculated as follows:

Crystallinity calculation: Xc ¼ Fc/(Fc þ Fa) � 100%,

where Fc was the crystalline area, Fa was the amorphous

area, and Xc was the crystallinity [14].

2 T. Huang et al. Starch/Starke 2012, 00, 1–9


2.5 Differential scanning calorimetry (DSC)analysis

Starch gelatinization was analyzed by DSC. Experiments

were carried out on a DSC-204-F1. Samples of 10 mg,

which were taken from the flour–water (1:2, w/w) suspen-

sions were sealed hermetically in aluminum crucible and

heated from 30 to 1208C at 108C/min. An empty aluminum

crucible was used as a reference. All tests were carried

out under N2 atmosphere. The starch gelatinization

parameters in the DSC thermogram included the onset

temperature (T0), the conclusion temperature (Tc),

the peak temperature (Tp), and phase transition enthalpy

DH [15].

3 Results and discussion

3.1 SEM analysis

Rice of different species possesses distinguishing AC and

the SEM photographs of its particle surface morphology

were shown in Fig. 1. The particle size of rice starch was

about 15–20 mm, and most of the starch granules were

irregular polygon with significant edges and corners

(Fig. 1). The first column showed the appearance of large

pores and cavities. A comparison of the numbers of

pores and cavities of rice manifest the fact that Enuo9

(Amylose11.6)>Guangliangyou558 (Amylose24.00)>

Yangliangyou419 (Amylose28.00). This phenomenon

can also be observed in the other two columns. These

pores and cavities may have osmosis effect when the

starch was gelatinized, because it facilitates the penetra-

tion of water and the leaching of amylose, which directly

leads to the swelling of rice starch granule. Meanwhile, the

fact was consistent with the report that starch granules of

rice with high AC possess more pores and cavities than

those with low AC [16].

Therefore, starch granules of Enuo9 (Amylose11.6)

expanded easily, followed by Guangliangyou558

(Amylose24.00), and Yangliangyou419 (Amylose28.00)

ranks the third. In terms of swelling ratio (SR) and

water absorption ratio (WAR) of rice, Enuo9>

Guangliangyou558>Yangliangyou419; in terms of HRD,

however, the order was opposite, which was in accordance

with the result of the report [10].

Figure 1. SEM image of rice powder (SEM4000 of the first column showed the surface of starch grains. SEM4000 of themiddle column mean the surface of a single particle of samples. SEM500 of the third column showed the surface of starchgrains. 4000, 500 means magnification.

Starch/Starke 2012, 00, 1–9 3


1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

R T 5 0 6 0

7 0 8 0 9 0

1 0 0

Enuo9 (Amylose11.60)

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

R T 5 0 6 0

7 0 8 0 9 0

1 0 0

Guangliangyou558 (Amylose24.00)

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0 1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

1 4 0 0 1 2 0 0 1 0 0 0 8 0 0 6 0 0 4 0 0

² ¨Ê ý

R T

²¨ Ê ý

5 0

² ¨Ê ý

6 0

² ¨Ê ý

7 0

² ¨ Ê ý

8 0

² ¨Ê ý

9 0

² ¨Ê ý

1 0 0

Yangliangyou419 (Amylose28.00)

Figure 2. FT-IR spectrum of rice powder at different temperatures (left top to bottoem: room temperature, 50, 60, 70, 80, 90,1008C).



3.2 FT-IR analysis

The A band at 1047 and 1022/cm were associated with the

ordered and amorphous structures of starch, respectively.

The changes in the intensity of these bands were strongly

associated with the alterations in the macromolecular

order [6, 17–19].

The ratio of A band at 1047 and 1022/cm was used to

quantify the degree of crystallization in starch samples.

The IR spectrum of all starch varieties were studied and

the ratio of A at 1047 and 1022/cm were calculated. A clear

segregation was found existing between the rice samples.

The ratio increased as the crystalline region expanded [6,

17, 18], therefore, the A1047/A1022 can be expressed as

the degree of crystallinity in rice starch.

The FT-IR spectrums of three kinds of rice starch (RT,

50, 60, 70, 80, 90, 1008C) were shown in Fig. 2. Peakfit

software was used to deconvolute IR spectrum, and the

peak area of 1047 and 1022/cm were used to analyze

variation trend of the ratio. It is also the variation trend of

crystalline and amorphous region. The ratio of deconvo-

luted crystalline and amorphous region during the heating

process was shown in Fig. 3A.

As it was shown in Fig. 3A, during the temperature-

changing (RT, 50, 60, 70, 80, 90, 1008C) heating process,

the ratio of Enuo9 (Amylose11.6) decreased the

most, reducing from 0.96 to 0.64, Guangliangyou558

(Amylose24.00) follows, diminishing from 0.98 to 0.79,

and Yangliangyou419 (Amylose28.00) dropped the least,

reducing from 0.82 to 0.72. It was demonstrated that the

change in the proportion of crystalline region and non-

crystalline region is related to the AC of rice, because

the high AC can prevent the structural damage of starch

crystal in the heating process, which was in accordance

with the literature [20]. It also showed that the intensity of

the infrared absorption peak varies as the rice starch

changes.

The variation trends of the FT-IR peak of the three

kinds of rice starch were shown in Fig. 3B. The absorption

peak of crystalline structure (1047/cm) shifted to a

higher wave number in the process of gelatinization,

and there was a slight or not significant change in the

non-crystalline area (1022/cm). The peaks of different

cultivars of rice were almost the same in crystalline and

non-crystalline area at RT, while a certain difference really

exists after heating. The change of peak position in the

crystalline area was bigger than that of non-crystalline

area.

3.3 XRD analysis

The wide-angle XRD diffractograms for three kinds of rice

starch in heating process (RT, 50, 60, 70, 80, 90, 1008C)

were shown in Fig. 4. The starch granule was a natural

polycrystalline system, constituted by the crystallization

phase and amorphous phase. XRD has been generally

used to analyze starch crystalline and amorphous areas, to

further study the crystallization structure and characteristic

of starch granules, and to evaluate the changes of starch-

related properties.

Rice samples at RT showed several diffraction peaks

around 2u ¼ 15.7, 18, and 238,which were typical patterns

of A-crystalline and the crystal structure had no change,

which was consistent with what Kim et al. [15] had reported

that raw rice starch was all A-crystalline type. But the

diffraction peak gradually weakened in the heating proc-

ess, and nearly disappeared when temperature reached

908C, which means that the crystal structure disappears

completely. This was consistent with what Mahanta and

Bhattacharya [21] had found that the A-crystalline type will

Figure 3. (A) FT-IR peak area ration of rice powder at different temperatures. (B) FT-IR peak point of rice powder.



0

200

400600

8001000

1200

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nsity

2 Theta

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nsity

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Yangliangyou419 (Amylose28.00)

Enuo9 (Amylose11.60)

Guangliangyou558 (Amylose24.00)

0

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400600

8001000

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0100200300400500600700800900

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10 20 30 40 50 600

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10 20 30 40 50 600

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10 20 30 40 50 600

10 20 30 40 50 600 10 20 30 40 50 600

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2 T heta10 20 30 40 50 600

2 T heta10 20 30 40 50 600

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10001200

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200300

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nsity

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Figure 4. XRD spectrum of rice pow-der (left top to bottom: room tempera-ture, 50, 60, 70, 80, 90, 1008C).



weaken after slightly cooking, and the crystal structure will

disappear completely after over-cooking.

A comparison of the decreasing speed of peaks of

the three diffractograms revealed that Enuo9 (Amylose

11.6) abated with the greatest speed at 70–808C,

Guangliangyou558 (Amylose24.00) decreased with

a medium speed at 808C, and Yangliangyou419

(Amylose28.00) decreased with the least speed at 80–

908C. These facts indicated that the increase of AC could

slow the weakening of the characteristic diffraction peak,

which was in accordance with the FT-IR result.

The variation trend of crystallinity of the three kinds

of rice during heating process of variable temperature

(room temperature (RT), 50, 60, 70, 80, 90, 1008C) was

shown in Fig. 5. The crystallinity of Enuo9 (Amylose11.6)

decreased fastest from (38.09%, RT) to (5.46%, 1008C),

Guangliangyou558 (Amylose24.00) decreased followed

from 32.19 to 5.99%, while Yangliangyou419

(Amylose28.00) reduced the minimum degree from

35.51 to 9.59%. This was in accordance with the variable

trend of the ratio of crystalline and amorphous region. It

indicated that the higher AC prevents the damage of starch

crystal in the heating process, which was conformable to

the report [20].

XRD crystallinity of rice blends was shown in

Table 1. Enuo9 and Yangliangyou419, Enuo9 and

Guangliangyou558, Guangliangyou558 and Yanglian-

gyou419 (1:1) were mixed into rice blends flour at RT,

and the crystallinity of these were 0.369174, 0.372755,

and 0.345025, which was the simple combination of

the original cultivars, without any strengthening or

weakening.

Enuo9 and Yangliangyou419 with significant differ-

ences of AC (1:1) were mixed into rice blend flour, and

the crystallinity was 0.067475, 1008C, while the crystal-

linity of Enuo9 and Yangliangyou419 were 0.054579 and

0.095934 at 1008C, respectively, which indicated it was

also a simple combination of the original cultivars in heat-

ing process, without any strengthening or weakening.

3.4 DSC analysis

DSC was commonly used for estimating the thermal prop-

erties of the starch. Gelatinization enthalpy refers to

energy required for the rice starch granules to be gelati-

nized completely, unit is J/g. Figure 6 presented DSC

thermogram of different kinds of starch granules, DSC

parameters were shown in Table 2. It indicated that

the DSC endothermal peak of Guangliangyou558

(Amylose24.00) occurred first at the lowest temperature

and enthalpy, probably because endotherm (energy)

required for the melting of crystalloid was the lowest.

The order of the melting temperature and enthalpy of rice

samples increased as follows: Enuo9 (Amylose11.6)>

(Amylose28.00)> Guangliangyou558 (Amylose24.00).

The order of melting temperature and enthalpy was con-

sistent with the crystallinity content in the rice samples,

which was in accordance with XRD analysis. In addition, it

also manifested the fact that AC was not relevant with the

Figure 5. XRD crystallinity of rice powder at varioustemperatures.

Table 1. XRD crystallinity of rice blend

1:1 Enuo9 Guangliangyou558 Yangliangyou419

Enuo9 0.380853 0.372755 0.369174Guangliangyou558 0.372755 0.32194 0.345025Yangliangyou419 0.369174 0.345025 0.355094

Figure 6. DSC curve of original rice and rice blend.



gelatinization temperature and enthalpy, which was

consistent with report [22].

Analysis from the figure pointed out that DSC curves,

Gelatinization temperature and Gelatinization enthalpy of

rice blends mixed by Yangliangyou419 (Amylose28.00)

and Enuo9 (Amylose11.6) (1:1) was the simple combi-

nation of the original cultivars without any strengthening

or weakening.

4 Conclusions

The gelatinization properties of rice have been investi-

gated in the simulated cooking process and the relation-

ship between AC and gelatinization property has been

discussed in the present work. New insights into the mech-

anism of edible quality of rice are provided in our result.

SEM analysis has been presenting that the starch

granule of rice with low AC show more pores and cavities

than those with high AC. These pores and cavities may

have osmosis effect when the starch is gelatinized,

because this facilitates the penetration of water and the

leaching of AM, which directly leads to the swelling of rice

starch granule. In the previous theoretical work [10], this

has been verified by the experimental results of rice HRD,

swelling volume and heating water absorption.

FT-IR analysis of variable temperatures has been pre-

senting that the change in the proportion of crystalline area

to non-crystalline area is related to the AC of rice, because

higher content of AM may prevent structural damage of

starch crystal in the process of heating, which was in

accordance with the previous report. XRD analysis has

been presenting that the increase of AC can slower the

weakening of the characteristic diffraction peak, and the

crystallinity of the rice with higher AC changed little in

the process of gelatinizing, which was in accordance with

FT-IR result, and it indicated that the higher AC can prevent

the structural damage of starch crystal in the process of

heating, which was conformable to the literature [20].

The crystal properties and thermal characteristics of

rice blend flour during the heating process compromise

between that of the original cultivars without any strength-

ening or weakening.

At present, the discussion of mechanism is only being

at an initial level, therefore, more extensive methods are

needed to explore the profound mechanism from the

microscopic point of view.

Financial support for this work was from contract grant

sponsors: The National Natural Science Foundation of

China (Grant No. 31071607).

The authors have declared no conflict of interest.

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Table 2. DSC parameter of original rice and rice blend

Sample T0 (8C) Tp (8C) Tc (8C) DT (8C) DH (J/g)

Enuo9 (Amylose11.60) 72.1 76.1 83 10.9 3.167Guangliangyou558 (Amylose24.00) 67.7 71 74.5 6.8 2.519Yangliangyou419 (Amylose28.00) 71.2 76.4 84.3 13.1 3.073Enuo9/Yangliangyou419 72.4 76.3 80.9 8.5 3.051



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study on gelatinization property and edible quality mechanism of rice

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