Accurate Measurement of Pasting Temperature by the Rapid Visco Analyser a Case Study Using Rice
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Transcript of Accurate Measurement of Pasting Temperature by the Rapid Visco Analyser a Case Study Using Rice
Rice Science, 2008, 15(1): 69–72Copyright © 2008, China National Rice Research Institute. Published by Elsevier BV. All rights reserved
Accurate Measurement of Pasting Temperature by the Rapid Visco-Analyser: a Case Study Using Rice Flour
BAO Jin-song (Institute of Nuclear-Agricultural Sciences/Key Laboratory of Chinese Ministry of Agriculture for Nuclear-Agricultural Sciences,
College of Agriculture and Biotechnology, Zhejiang University, Hangzhou 310029, China)
Abstract: Pasting properties are among the most important characteristics of starch, determining its applications in food
processing and other industries. Pasting temperature derived from the Rapid Visco-analyser (RVA) (Newport Scientific), in
most cases, is overestimated by the Thermocline for Windows software program. Here, two methods facilitating accurate
measurement of pasting temperature by RVA were described. One is to change parameter setting to ‘screen’ the true point
where the pasting viscosity begins to increase, the other is to manually record the time (T1) when the pasting viscosity begins
to increase and calculate the pasting temperature with the formula of (45/3.8)×(T1–1)+50 for rice flour. The latter method
gave a manually determined pasting temperature which was significantly correlated with the gelatinization temperature
measured by differential scanning calorimetry.
Key words: rice; starch; gelatinization temperature; pasting temperature; methodology
In addition to amylose content, pasting and gelatinization
properties are among the most important physicochemical
properties of starch that determine its applications in food industry
and other uses [1]. Among rice grain quality, amylose content is
believed to be the most important parameter in determining the
eating and cooking quality of cooked rice [1-3], and it is agreed
that pasting viscosity properties and gelatinization temperature
(GT) also contribute to differences in cooked rice quality [4-5].
Pasting viscosity properties have been used to predict the
end-use quality of various products, e.g. cooked rice texture [4,6]
and noodles [7]. In many food industries, analysis of pasting
viscosity and gelatinization temperature is still necessary for
samples at different stages of processing.
Pasting properties of starches are measured by using
various instruments such as Rapid Visco Analyser (RVA,
Newport Scientific, Warriewood, Australia), Micro Visco-
Amylograph (Brabender, Duisberg, Germany), etc [8]. GT is the
critical temperature at which starch granules irreversibly lose
their birefringence and crystalline order during heating. GT can
be directly measured under a polarized light microscopy with a
heating stage to record the temperature when the birefringence
is lost. GT can also be measured by differential scanning
calorimetry (DSC) [9], or indirectly by the alkali spreading
value test for rice grains [10]. Some studies also measured the
pasting temperature (PT) of starch from RVA analysis [3, 6, 8, 11].
If the PT obtained from RVA were equivalent to the GT from
DSC, information on pasting viscosity and gelatinization temperature
Received: 2 August 2007; Accepted: 9 October 2007Corresponding author: BAO Jin-song ([email protected]) This is an English version of the paper published in Chinese in ChineseJournal of Rice Science, Vol. 21. No. 5, 2007, Pages 543–546.
could be simultaneously obtained from a single test on the RVA,
thus saving time and resources. Unfortunately, the PT measured
from RVA is always overestimated, being much higher than the
GT derived from DSC. In some cases, the RVA derived PT of
rice samples was higher than 90°C [3, 6]. Hence, the PT from
RVA will be misleading if it is not interpreted properly. In the
present paper, we report how to accurately estimate the
gelatinization temperature using RVA.
MATERIALS AND METHODS
Rice materials
A total of 15 rice varieties (or breeding lines) representing
a wide range of amylose content (2% to 30%) and gelatinization
temperature were used in this study. The rice was grown in
Hainan Province, China from November 2003 to April 2004.
Rough rice grains were dehulled, and milled to white rice with
a Satake mill (Satake Corp. Japan) and then ground to flour
with a Cyclone sample mill (UDY Corp., Fort Collins, CO).
The flour was further passed through a 100-mesh sieve prior to
analysis.
RVA measurement
Rice flour pasting properties were determined using a
Rapid Visco-Analyzer model 3D (RVA) (Newport Scientific,
Warriewood, Australia) with the software program Thermocline
for Windows (TCW) according to AACC method 61-02 [12].
Each rice sample (3 g, 12% m.b.) was mixed with 25 g of
distilled water in an RVA sample canister. The idle temperature
was set at 50°C, and the following 12.5-minute test profile was
run: (1) held at 50°C for 1.0 min, (2) linearly ramped up to
70 Rice Science, Vol. 15, No. 1, 2008
95°C in 3.8 min, (3) held at 95°C for 2.5 min, (4) linearly
ramped down to 50°C in 3.8 min and (5) held at 50°C for 1.4
min. The peak viscosity, holding viscosity, final viscosity, and
pasting temperature were determined by the analysis window
of TCW. In the program, the formula to measure pasting
temperature is TempAtViscRate (T1,T2,.Tinc,Vinc), which
means that the temperature (°C) when the rate of change in
viscosity (Vinc/Tinc) is first achieved between T1 (min) and T2
(min) of the curves. The viscosity is either in RVA arbitrary
unit (RVU) or centiPoise (cP). For rice flour, the recommended
total test time is generally 12.5 min (AACC 2000), thereby the
first two parameters (T1 and T2) of the formula are generally
set as (2, 7), whereas the latter two parameters (Tinc and Vinc)
can be changed.
DSC analysis
The gelatinization temperatures of the rice flour samples
were measured with a DSC 2920 Modulated DSC thermal
analyser (TA Instruments, Newcastle, DE) equipped with DSC
standard and dual sample cells. Rice flour (2.0 mg) was weighed
into an aluminum pan, 6 µL distilled water was added, and the
pan was sealed hermetically with a lid. After equilibration at
room temperature for 1 h, the sample was heated at a rate of
10°C/min from 30°C to 110 °C. A sealed empty pan was used
as a reference. Onset (To), peak (Tp), and completion (Tc)
temperatures of gelatinization were calculated by a Universal
Analysis Program, Version 1.9D (TA Instruments, Newcastle, DE).
Statistical analysis
Student’s t-test for comparing the means of the paired data
and analysis of correlation coefficient were carried out in
Microsoft Excel (Microsoft Corp, Seattle, WA).
RESULTS AND DISCUSSION
According to the software formula setting, the pasting
temperature (PT) was recorded when the rate of change viscosity
above the set point was first achieved. In many cases, the
viscosity increased rapidly after initial rise, so the formula given
by the software, such as TempAtViscRate (2,7,.2,24), accurately
measured the PT (Fig. 1-A). For example, the software gave the
samples BP003, BP004 and BP095 the PTs with less than 2°C
deviation when different parameters were tried (Table 1). In
some cases, wide deviations in the PTs were found when
different formulas were tried. For example, the formula
TempAtViscRate (2,7,.1,36) gave BP530 and BP547 the PTs
higher than 88°C (Table 1), whereas the TempAtViscRate
(2,7,.1,10) formula gave them around 73oC (Table 1). The
reason was that the pasting viscosity was increasing at a low
rate, even lower than the set point for a long time (Fig. 1-B to
F). For example, if a sample’s pasting viscosity increased at a
constant rate of 18 cP/s between the time 2 min to 7 min during
test, no PT would be recorded with formula TempAtViscRate
(2,7,.1,36) or TempAtViscRate (2,7,.1,24) because the actual
rate was always less than 36 or 24 cP/s. Thus, the recorded PT
would gradually decline as the set rate declined as shown in Fig.
1-B to F. However, too small a change rate setting would also
result in incorrect PT, such as TempAtViscRate(2,7,.1,10) gave
BP005 66°C, much lower than the true value (Table 1).
Because of genotypic differences in pasting behavior, accurate
Fig. 1. Typical pasting profile of rice flour tested on a Rapid Visco-analyser. A, PT derived from the program formulae of TempAtViscRate (2,7,.2,24) for rice BP003; B to F, PT derived from various program formula of
rice BP025; B, TempAtViscRate (2,7,.1,36); C, TempAtViscRate (2,7,.1,24); D, TempAtViscRate (2,7,.1,18); E, TempAtViscRate (2,7,.1,12); F,TempAtViscRate (2,7,.1,10). Peak, Peak viscosity; Hold, Holding viscosity; Final, Final viscosity; PT, Pasting temperature.
Vis
cosi
ty
(cP
)
V
isco
sity
(cP
)
Tem
pera
ture
(°C
)
T
empe
ratu
re (
°C)
Vis
cosi
ty (
cP)
Time (min) Time (min)
Temperature
Temperature
Viscosity
Viscosity
BAO Jin-song. Accurate Measurement of Pasting Temperature by the Rapid Visco-Analyser: a Case Study Using Rice Flour 71
automatic measurement of PT by a single formula was
impossible. To analyze with different formulae and check
whether the PT was determined at the proper point would help
to obtain a correct result for a specific pasting profile. Two
inferences could be drawn. One is that an accurate PT is easier
to be obtained for higher viscosity samples because of a
generally rapid increase in viscosity for these samples. The
other is that measurement of PT will be affected by starch or
flour concentrations. Lower concentration of a sample results in
higher PT when measured by the software formula though it is
actually low in gelatinization temperature, whereas higher
concentration leads to more accurate measurement of the PT
because of the rapid increase in viscosity. Varavinit et al [3] used
1.5 g rice flours instead of 3.0 g to test pasting properties, so
the high PTs (>90°C) might result from the low concentration.
PT could be measured by inspection of individual curves
to determine the point at which the pasting viscosity began to
increase (Fig. 1-B). Since the temperature was increased
linearly from 50°C to 95°C in 3.8 min during pasting and was
held at 50°C for 1.0 min before increasing the temperature, the
PT could be calculated by the formula, PTm = (45/3.8)×
(T1–1)+50, where T1 is the time when the pasting viscosity
began to rise (Table 1). In the TCW software, the time at the
point when the mouse arrow lies in the curve will be displayed
when the ‘Show Cursor Coordinates’ is chosen in the ‘Options’.
This method was very accurate, because in TCW, one can
enlarge the profile so as to locate the point at a right place. We
recorded the time for all 15 samples and calculated the PT
(Table 1). As a result, the manually calculated PTs (PTm) were
significantly correlated with those from DSC measurements,
whereas all other software formula derivatives gave poor
correlation with DSC parameters (Table 2). TempAtViscRate
(2,7,.2,24), TempAtViscRate (2,7,.1,12) and TempAtViscRate
(2,7,.1,10) gave relatively more accurate PT because of their
higher correlation with DSC parameters (Table 2).
Under the assumption that the two paired data had the
same mean, the Student’s t-test indicated that PTm was
significantly different from To (P<0.0001), Tp (P<0.01) and Tc
Table 1. Pasting temperatures of rice flours derived from different methods.�
PT a (˚C)� PTm b� � DSC c (˚C)�
Sample�(2,4) d (2,24) (2,36) (1,36) (1,24) (1,18) (1,12) (1,10)
Time(min)
PT (˚C)
To Tp Tc
BP003 77.7� 76.7� 77.7� 78.4� 77.7� 77.7� 77.7� 76.7� 3.17 75.7� 71.2� 75.2 81.0
BP004 77.6� 76.8� 77.6� 78.4� 77.6� 77.6� 76.8� 76.8� 3.28 77.0� 72.4� 75.8 81.2
BP005 79.9� 79.2� 79.2� 79.9� 79.9� 79.2� 75.2� 66.0� 3.47 79.2� 74.4� 78.9 83.7
BP010 85.4� 72.9� 72.9� 86.1� 73.5� 73.5� 70.6� 67.4� 2.50 67.8� 58.3� 67.0 76.1
BP011 79.1� 78.3� 79.1� 79.9� 79.9� 79.1� 78.3� 75.8� 3.43 78.8� 74.8� 79.4 84.6
BP025 83.8� 71.9� 76.0� 87.9� 79.1� 72.9� 71.9� 70.6� 2.73 70.5� 63.0� 69.2 76.1
BP026 73.6� 70.5� 71.3� 74.5� 74.5� 71.3� 70.5� 70.5� 2.75 70.7� 62.9� 69.6 78.0
BP086 83.0� 69.1� 81.6� 87.2� 82.3� 81.6� 69.8� 68.2� 2.42 66.8� 58.1� 65.2 72.6
BP095 76.8� 76.0� 76.8� 77.6� 77.6� 76.8� 76.8� 76.0� 3.20 76.1� 70.6� 75.3 81.2
BP133 79.9� 66.8� 78.3� 82.9� 79.1� 66.8� 66.8� 66.0� 2.38 66.4� 56.3� 63.4 70.9
BP225 69.7� 69.0� 69.0� 71.4� 69.7� 69.7� 69.0� 68.2� 2.55 68.4� 62.5� 70.3 77.3
BP420 85.4� 80.7� 84.0� 86.2� 84.6� 81.5� 80.7� 70.5� 2.48 67.6� 58.7� 65.6 72.9
BP530 87.8� 77.4� 83.8� 88.6� 87.2� 83.0� 78.3� 73.6� 2.75 70.7� 62.9� 69.2 76.1
Bp547 87.2� 84.0� 85.4� 89.5� 86.1� 84.6� 72.9� 72.9� 2.77 70.9� 62.7� 68.9 75.8
Bp551 82.2� 70.5� 77.6� 84.5� 81.5� 72.9� 69.7� 69.7� 2.63 69.3� 59.2� 66.0 73.1a PT was pasting temperature derived from program software formula, TempAtViscRate (2,7,.Tinc,Vinc); b PTm was pasting temperature derived from manual location of the time when the viscosity began to rise; c Differential scanning calorimetry: To, Onset temperature; Tp, Peak temperature; Tc, Completion temperature; d This was set in the RVU mode, whereas others were in cP mode.
Table 2. Correlation coefficients for pasting temperatures derived from different methods with DSC values a.
Parameter (2,4) b (2,24) (2,36) (1,36) (1,24) (1,18) (1,12) (1,10) PTm
To� -0.35� 0.49� -0.02� -0.46� -0.11� 0.28� 0.59*� 0.60*� 0.99**�
Tp� -0.38� 0.47� -0.09� -0.49� -0.18� 0.25� 0.56*� 0.54*� 0.97**�
Tc� -0.40� 0.44� -0.18� -0.52*� -0.26� 0.20� 0.52*� 0.52*� 0.94**�
* and ** are significant at P<0.05 and P<0.01, respectively; a Differential scanning calorimetry: To, Onset temperature; Tp, Peak temperature; Tc, Completion temperature; b This was set in the RVU mode, whereas others were in cP mode.
72 Rice Science, Vol. 15, No. 1, 2008
(P<0.0001). However, when the difference between two paired
data was set to 1°C, the PTm was not significantly different
from Tp (P = 0.71), but it was still significantly different from
To and Tc (P<0.0001), indicating that the mean PTm (71.7°C)
was only 1°C higher than the mean Tp of DSC (70.6°C).
Our analysis only focused on the measurement of PT of
rice flour tested according to the AACC method 61-02; whether
other samples or other methods will encounter the same
problem is not known. The manually obtained PT should
always resolve the problem, but the formula to calculate the PT
could be reestablished for that specific method.
CONCLUSIONS
Pasting temperature measured by RVA does not reflect the
true gelatinization temperature, such as measured by DSC.
Changing parameters in the analysis program could increase
the measurement accuracy but still gave great deviation for
some samples. Inspecting the curves to record the time (T1)
when the pasting viscosity began to rise and calculating the
pasting temperature by a specific formula, such as
(45/3.8)×(T1–1)+50 for rice flour can measure the pasting
temperature (estimate gelatinization temperature) very accurately.
The results also indicated that the pasting temperature from
RVA was 1°C higher than peak temperature of DSC.
ACKNOWLEDGEMENTS
This research was financially supported in part by the
National High Technology Development Project of China
(Grant No. 2006AA10Z193), the National Natural Science
Foundation of China (Grant No. 30300227), and the Science
and Technology Department of Zhejiang Province (Grant No.
2007C32014).
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