International Journal of Food Processing Technology, 2014, 1, 10-17 10

Microstructure of an Extruded Third-Generation Snack Made from

a Whole Blue Corn and Corn Starch Mixture

R.O. Navarro-Cortez1, E. Aguilar-Palazuelos1, J.J. Zazueta-Morales1, J. Castro- Rosas2,

J. Hernández-Ávila3 and C.A. Gómez-Aldapa2, *, F.S. Aguirre-Tostado 4,

1
Universidad Autónoma de Sinaloa, Facultad de Ciencias Químico-Biológicas, Maestría en Ciencia y
Tecnología de Alimentos, Boulevard Américas, Culiacán, Sin, C.P. 82000. México
2 3
Universidad Autónoma del Estado de Hidalgo, Área Académica de Química, Área Académica de Ciencias
de la Tierra y Materiales, Ciudad del Conocimiento, Carretera Pachuca-Tulancingo Km. 4.5, Col. Carboneras,
Mineral de la Reforma, Hgo, C.P. 42184. México
4
Centro de Investigación en Materiales Avanzados, S.C., Alianza Norte 202,Parque de Investigación e
Innovación Tecnológica,Apodaca, NL, C.P. 66600, México
Abstract: Blue corn is a potential material for expanded snack production. Whole blue corn meal was mixed with corn
starch and processed by extrusion to produce a third-generation snack. Optimum extrusion conditions were calculated
with the response surface methodology using expansion index (EI), penetration force (PF), specific mechanical energy
(SME) and total anthocyanins content (TAC). Optimum conditions (zone 1, 67°C; coo king zone, 123°C; zone 3, 75°C;
feed moisture, 24.6%) were used to extrude the mixture in a single-screw extruder, and EI,PF,SME and TAC of the
expanded pellet were compared against predicted optimum values. Starch structural changes in pellets and expanded
were analyzed with DSC, viscosity profiles, x-ray diffraction and SEM. Extruded pellet did not differ (p>0.05) from the
predicted. However, TAC was lower (p<0.05) in the expanded pellet. Structural analyses showed damage starch
granular structure during extrusion and pellet expansion. Blue corn is a promising material for production of third-
generation snacks.

Keywords: Extrusion, Expansion, Starch microstructure, Differential scanning calorimetry, Anthocyanins.

INTRODUCTION and starch digestibility, solubilizing insoluble fiber, and

inactivating toxins, anti-nutritional factors and
Over the last thirty years, worldwide obesity undesirable enzymes such as lipo-oxygenases and
incidence has increased substantially, making it one of peroxidases [6]. Extrusion of meals and other products
the fastest growing diseases in the world. Data of with starch in their structure (e.g. cereals) is widely
World Health Organization (WHO) in the year 2012, 44 used in the food industry to produce snack foods [7].
millions of child in the world below 5 years had
overweight or obese, one in six adult in the world was White corn and yellow corn exhibit good expansion
obese, one in ten was diabetic, and one in three had characteristics. Blue corn may also therefore have
raised blood pressure. The American continent has the good physical and technological characteristics for
highest obesity rates (26% of adults) [1]. In Mexico, snack food production. When used in the manufacture
obesity is the principal factor contributing to develop- of a second-generation snack with added calcium
ment of chronic, non-communicable diseases such as hydroxide, it exhibited good technological characteris-
diabetes mellitus and cardiovascular diseases, the two tics for extruded snack production [8]. Blue corn con-
main causes of death in the country [2,3]. In 2008, the tains anthocyanins, the most frequent being cyanidin 3-
costs attributable to obesity in Mexico totaled 42 billion glucoside [9,10]. Anthocyanins are natural pigments
pesos, but these could increase to 101 billion pesos by safe for human consumption that can be used as food
2017 [4]. Recent data place obesity and overweight additives. Interest in anthocyanins as a promising
prevalence in Mexico at 71.28%, which represents 48.6 alternative food coloring has increased in response to
million people [5]. In response to this public health cha- their coloring properties and potential health benefits
llenge, many snack manufacturers have begun modify- [11]. They are exceptionally potent oxygen radical
ing production processes to create low-fat products. scavengers with known beneficial effects in diseases
Extrusion is very useful in producing low-fat improving outside the cardiovascular system, but may also
snack foods and has the added advantages of protein provide some benefits in heart disease [12].

*
Address correspondence to this author at the Universidad Autónoma del Est- The present study objective was to determine opti-
ado de Hidalgo, Área Académica de Química, Ciudad del Conocimiento, Carr- mum processing conditions for third-generation snacks
etera Pachuca-Tulancingo Km. 4.5, Col. Carboneras, Mineral de la Reforma,
Hgo, C.P. 42184. México ; Tel: +52 (771) 7172000 Ext. 6501; using a whole blue corn and corn starch mixture, and to
Fax: +52 (771) 7172000 ext. 6502.E-mail: [email protected]

© 2014 Cosmos Scholars Publishing House

Development of a Third-Generation Snack with Blue Corn and Corn Starch International Journal of Food Processing Technology, 2014, Vol. 1, No. 1 11

evaluate anthocyanin content and starch structural Extrusion Process

damage after extrusion and microwave expansion.
A single-screw laboratory extruder (Brabender
MATERIALS AND METHODS Instruments Inc., model 20DN/8-235-00, CW, Duisburg,
Raw Materials Germany) was used with a 19 mm internal barrel
diameter, 20:1 length/diameter ratio, a 2:1 screw
Commercially available blue corn (Zea mays L. var. compression ratio and a rectangular matrix with a 20 x
chalqueño) was purchased in a local market in the 1.5 mm exit aperture area. The extruder barrel was
State of Mexico. Normal corn starch was purchased divided into two independent heating zones (feed and
from Grupo Emsiana S.A. de C.V. (Puebla, Mexico). cooking), using air circulation to maintain an accurate
temperature. Feed zone temperature was 67±3°C,
Meal Production
cooking zone temperature was 122±3°C and exit matrix
Blue corn grain was ground in a hammer mill with a temperature was 75±3°C. The blue corn/corn starch
1 mm mesh. The resulting meal was mixed with normal mixture was fed into the extruder at a 1.56 kg/h feed
corn starch at a 65:35 ratio and 0.1% monoglycerides rate with an 80 rpm screw speed, under these
added to improve final product appearance. conditions the mixture of blue corn and starch flowed
continuously into the extruder and the product had
Process Optimization
good appearance. Cooking zone temperature (123°C)
Optimization of the manufacturing process for a and mixture feed moisture content (24.6%) were
third-generation snack from whole blue corn and corn selected from the optimization graph (Figure 1). The
starch was done using the response surface resulting products were analyzed to quantify their
superposition methodology. The response variables physical and chemical characteristics.
used in the optimization of the extrusion process were
Characterization of Extruded Products
the expansion index (EI), penetration force (PF),
specific mechanical energy (SME) and total content
The strips produced in the extrusion process were
anthocyanins (TAC). These responses were selected
based on the most important traits required in a third- cut into 3 cm-long pellets and expanded in a
®
generation snack. The SME was used to evaluate microwave oven (LG brand, model R-501CW, 900
process energy expenditure and indirectly determine W/2450 Hz power, Beijing, China) for 26s; were tested
starch granule damage. Total anthocyanins content different times of expansion in the microwave oven 20,
(TAC) was quantified due to their ability to neutralize 23, 26, 29 and 32s, shorter times to 26s the pellet not
damaging reactive species in the human organism. expanded complete and times higher to 26s the pellet
Once the optimum processing area was calculated, the was burning. Randomly were selected lots of 30 pellets
central point was taken and these optimum extrusion and were expanded. Expansion index was measured
conditions were tested experimentally. The design for the expanded pellets using the seed displacement
experimental used was a central composite rotatable method [13], with millet as the seed.
where was evaluated the effect of extrusion
temperature (98.79-141.21) and moisture feed (19.93- The force required to penetrate the expanded
34.07) (Table 1), on the responses variables EI, SME, product was measured with a penetrometer (Chatillón
FP and TAC. A linear regression analysis was TCD 200, Viennacourt, Lammas Road, Godalming,
conducted to relate each response with extrusion Surrey, UK). Expanded samples were placed horizon-
temperature and moisture feed. The response surface tally on a 1 cm thick plastic platform and penetrated
model used for each response was with main, with a 2 mm flat tip cylindrical probe. Probe descent
-1
interactions, and quadratic terms: rate was 0.83 mm.s , and maximum penetration
y =
0 +
1 x1 +
2 x2 +
12 x1 x2 +
11 x12 +
22 x22
distance was 3 mm. Thirty measurements were taken
per treatment and values reported as Newton’s (N).
Table 1: Rotatable Central Composite Design used to
Evaluate Responses for EI, PF, SME and TAC Specific mechanical energy is a numerical value
expressed as energy per weight unit (J/g). It is
Levels calculated from the torque (T) (N*m), screw speed (Ss,
Independent Variables -
-1 0 +1 +

rpm) and feed rate (F, g/min) values:

Temperature (°C) 98.79 105 120 135 141.21 SME=2TSs/F

Moisture feed (%) 19.93 22 27 32 34.07
12 International Journal of Food Processing Technology, 2014, Vol. 1, No. 1 Navarro-Cortez, et al.

Specific mechanical energy is defined as the net 5.6°C/min; and held at 50°C for 2 min (Newport-
mechanical energy per mass unit required by the Scientific 1992). The resulting viscosity profiles were
extruder to turn the screw, and provides data on used to measure initial viscosity (Vini); viscosity at 92°C
extruder operation [14]. (V92); minimum viscosity (Vmin) (i.e. the lowest viscosity
value during the 92°C constant temperature); and final
Total anthocyanins content was measured viscosity (Vfin) (i.e. maximum viscosity during cooling
according to Abdel-Aal & Hucl, 1999 [15]. Samples period). Retrogradation viscosity (Vr) (i.e. Vfin - Vmin)
containing 9-13% moisture were ground into meals and was calculated from these parameters [16].
passed through No. 60 mesh. From these meals, a 1 g
sample was placed in a 50 mL centrifuge tube with 8 Samples of the unprocessed meal, the pellet and
mL acidified ethanol (85 mL 95% EtOH + 15 mL 1.0 N the expanded product for each treatment were packed
HCl), the tube was manually agitated for 2 min and pH into a 0.5 mm deep glass slide and placed in a Rigaku
adjusted to 1.0 with a water distilled:HCl (1:1) solution. x-ray diffractometer (Ultima D/Max-2100, RigakuDenki
The tube was agitated for 30 min and pH readjusted if Co. Ltd, Japan). The X-ray source was CuK
with a
necessary. It was then centrifuged at 3220 x g for 30 wavelength of 1.5406°, 30kV, and 30 mA. Data were
min at room temperature, the supernatant completed to collected of 0-40° on a 2 scale (2 is the angle of
25 mL with acidified ethanol and absorbance read at diffraction to the incident beam)
535 nm using a spectrophotometer (UNICO SQ 2800,
NJ, USA). Acidified solvent was used as a blank. The Samples were analyzed with a scanning electron
absorbance value was inserted into this equation: microscope (INCAx-sight 6650, Oxford Instruments,
Abingdon, Oxfordshire, UK) equipped with a secondary
6
C=(A/E) x (TV/1,000) x MW x (1/SW) x 10 electrons detector. Ground samples (<60 mesh) were
placed in a PIN-type aluminum of 12 mm diameter
where previously prepared with double-sided carbon tape. For
-1 the blue corn / corn starch mixture, micrographs were
C = Total anthocyanins content (mg
kg ),
taken at 10 KV and 1200 magnifications, while for the
A = Absorbance at 535 nm,
pellets and expanded product they were taken at 67
E = Molar absorption coefficient (cyanidin 3-
-1 magnifications.
glucoside= 25,965cm L/mol),
TV = Total volume (mL) of anthocyanins extract, RESULTS AND DISCUSSION
MW = Molecular weight of cyanidin 3-glucoside
(449 g/mol), Optimization
SW = Sample weight.
Food processed by extrusion containing starch can
Samples were analyzed in a differential scanning expand from 2 to 9 fold, depending on starch type and
calorimeter (Mettler-Toledo, 822e, Switzerland), processing conditions, including temperature and
calibrated with indium. A microsyringe (Hamilton Com- moisture content. Optimization criteria were a minimum
pany, USA) was used to inject 16 mg distilled water to EI value of 4.1 and a maximum PF value of 13, both of
4 mg sample into a 40μL aluminium capsule. Capsules which are used for commercially available products.
were placed in a heating chamber ventilated with Based on reported SME values for blue corn products
nitrogen (20 mL/min), and analyzed in a range of 30 to (<250 kJ/kg) [8], maximum acceptable SME was fixed
130°C at the rate heating of 5°C/min. Enthalpy and at 200 kJ/kg. Minimum TAC was established as 70 mg
onset peak and final temperatures were measured with anthocyanins/kg sample, since this is the value
the STARe Thermal Analyzer ver. 8.1 software. recorded for blue corn and corn starch expanded
products with EI and PF values similar to those of
Viscosity of extruded products was measured at commercial snack products.
92°C with a Rapid Visco-Analyzer (RVA 3C, Newport
Scientific PTY Ltd., Sydney, Australia), following Optimum extrusion conditions for the third-
manufacturer instructions. Briefly, 2 g sample was generation snacks made from blue corn and corn
adjusted to 28 g with distilled water in an aluminium starch were 120-126 °C and 23.80-25.20% moisture
slide. The sample-water suspension was kept under content (Figure 1). The central point (123 °C, 24.6%
constant agitation and heated in the following moisture) was selected and validated experimentally.
sequence: 50°C for 1 min; heated to 92°C at 5.5 Predicted values for this point were EI = 4.10±0.04; PF
°C/min; held at 92°C for 5 min; cooling to 50°C at
Development of a Third-Generation Snack with Blue Corn and Corn Starch International Journal of Food Processing Technology, 2014, Vol. 1, No. 1 13

= 12.42±0.31 N; SME = 169.08±1.85 J/g; and TAC = Differential Scanning Calorimetry

71.09±1.10 mg anthocyanins/kg sample. Pellets
produced using the central point extrusion conditions Calorimetric techniques are used to study the
exhibited average values of EI = 4.47± 0.07; PF = structure and phase transitions in pure starch in food
11.45±0.49 N; SME = 185±5.5 J/g; and TAC = 61 ± systems, and help to identify structural changes caused
1.74 mg anthocyanins/kg sample. Only anthocyanin by heat and moisture during processing [20]. The DSC
content differed (p<0.05) between the central point and thermogram for the blue corn/corn starch meal showed
the experimental products. All other values did not values (onset = 64.4 ºC; peak = 69.45 ºC, end = 73.67
differ (p=0.05). Therefore, the model is effective for ºC) indicating the starch had not been submitted to
producing a third-generation snack using extrusion hydrothermal processing, exhibited no structural da-
technology. mage and had the capacity to form a gel in the pres-
ence of excess water and high temperature (Figure 2).
The pellet, and expanded product, not showed thermal
signal, meaning that their structures contained no
starch with a crystal organization. The thermomecha-
nical process completely gelatinized the starch,
probably degrading it by the applied shear force. These
results agree with the statement of Chinnaswamy and
Hanna [21] that processed starch does not exhibit a
gelatinization peak because the starch’s crystal
structure has been transformed or the starch
completely gelatinized. In a study of corn products
extruded at 90 and 100 °C, no endothermal peak was
observed since at these temperatures the starch is
completely gelatinized [22]. No thermal signal is
observed in extruded products with high EI values [23],
however, absence of a gelatiniza-
Figure 1: Optimum processing area (black zone) for a third tion peak does not guarantee that a starch has comple-
generation extruded snack made from a whole blue corn / tely lost its granular and crystalline structure [24].
corn starch mixture.

Anthocyanin Content

Anthocyanins content in the mixture was

248.67mg/kg mixture prior to extrusion. Processing
under the optimum conditions caused the loss of 75%
of anthocyanins, which was expected since antho-
cyanin degradation is a function of temperature and
exposure time [17]. These results are similar to those
for breakfast cereal made with extruded corn and blue-
berry or grape concentrates in which anthocyanin loss
was 70% in the samples containing grape and 90% in
those containing blueberry [18]. Use of raw materials Mix (CM+CS)
Pellet
20 40 60 80 100 120 140
with anthocyanins in their structure could be used to Expanded
Temperature ºC
produce colored products, thus reducing the need for
artificial colorings in extruded products and providing
health benefits. Anthocyanins are very effective at Figure 2: Differential scanning calorimetry thermograms for
- the whole blue corn (CM)/corn starch mixture (CS), extruded
trapping free radicals due to their OH groups, and
pellets and expanded products.
consequently can provide an anti-inflammatory effect,
protection against liver damage, reduction of blood Viscosity Profiles
pressure and improved vision [19]. Using higher screw
speed and feed moisture higher may help to retain Viscosity profiles are analyzed by adding water to
higher anthocyanin in the extrudate, due to a decrease ground or powdered products and monitoring changes
in the residence time in the extruder barrel.
14 International Journal of Food Processing Technology, 2014, Vol. 1, No. 1 Navarro-Cortez, et al.

in viscosity during a temperature cycle. Paste viscosity 8000 95

is another way of evaluating degree of degradation in 7000

90

starchy materials during thermal and mechanical treat- 6000

85

ments. Severe treatments destroy starch granular stru- 80

5000
cture, consequently diminishing hot paste viscosity 75

[25]. The viscosity values (Vini, V92, Vmin, Vfin and Vsetback) 4000 70

of the studied meal, pellets and expanded products 65

Viscosity (cP)
3000

Temperature ºC
60
confirm this since they indicate that starch granule inte- 2000
55
grity had been affected by the heat and shear force of 1000
50
extrusion (Table 2). This damaged the starch’s water P e lle t
0 45
absorption capacity at high temperatures, lowering its 0 400 800 1200 1600
E xpa nded
M ix (CM+ CS)
200 600 1000 1400
gelling capacity and consequently affecting paste vis- T e m pe ratura ºC
T im e (s)
cosity. In a study of puffed cereal grain meals, paste
viscosity decreased due to starch structural changes
[26]. There was a clear difference visible in the present Figure 3: Viscosity profiles for the whole blue corn (CM) /
corn starch (CS) mixture, extruded pellets and expanded
results between the paste forming capacities of the products.
native and processed starches. Processing also favor-
ed amylose precipitation, affecting Vr since a native or Native starches require water and heat to swell, a
unprocessed starch has a greater capacity to phenomenon, which favors hydrogen bond rupture and
retrograde. loss of packing among polymer molecules within the
granule. If it’s crystalline structure is broken by
Table 2: Viscosities at Different Heating Times for mechanical methods or heating in water, the granule
Whole Blue Corn/Corn Starch Mixture,
exhibits paste viscosity at cold temperatures, which is
Extruded Pellets and Expanded Products
indicative of severe starch granule disruption during
processing [28].
Viscosity (cP)
X-ray Diffraction
Material Vini V92 Vmin Vfin Vr

Mix (CM+CS) 76 4797 2825 6664 3839 At the 2
scale used here, the blue corn/corn starch
mixture exhibited XRD values of 14.92, 17.62 and
Extruded Pellets 220 824 617 878 261
22.76 º (Figure 4). These values correspond to an A-
Expanded type diffraction pattern found in cereal starches like
194 365 326 387 61
Products
those in the present study. Both the pellets and
V ini = Initial viscosity; V92 = 92 ºC viscosity; V min = Minimum viscosity; V fin expanded products had values of 13 and 20 °, the
= Final viscosity; Vr = Retrogradation viscosity.
latter corresponding to a V-type pattern indicating
amylose-lipids complex formation [28]. Extrusion
In the viscosity profiles, the meal exhibited viscosity
involves high temperatures, and at high temperatures
until heated, whereas the pellets and expanded
complexes may form between amylose and free lipids
products had water adsorption capacity when cold and in the raw material, which favor formation of type-II
developed viscosity, although with values lower than lipid-starch complexes [29]. These diffraction patterns
for the native starch (Figure 3). This agrees with have also been observed during amylose molecule re-
Becker et al. [27], who stated that thermal processing association into double helices within the starch’s
of starches produces a viscosity peak at cold three-dimensional network. These results also agree
temperatures, but when the starch is heated in water with those of Miyoshi [30], who observed peak
this peak is lower than in intact starch granules. In the formation in hydrothermally-treated corn and potato
present results, this behavior can be attributed to starches at a 2
angle of 19.5 º. This corresponded to
changes in starch internal structure caused by thermo- a V-type pattern caused by amylose complex formation
mechanical treatment of the blue corn/corn starch and amylose recrystallization. High temperatures can
mixture. In this restructuring, hydrophilic starch groups completely destroy starch structure, producing an
are exposed to water, and the principal changes occur amorphous state on XRD graphs, or can induce forma-
when granule crystalline regions become amorphous tion of a new structure [31]. Formation of starch/lipid
as the granule fuses, thus favoring water uptake in cold complexes is favored when lipid chains are small. For-
temperatures. mation of these complexes can provide health benefits
because it reduces the amount of lipids available for
Development of a Third-Generation Snack with Blue Corn and Corn Starch International Journal of Food Processing Technology, 2014, Vol. 1, No. 1 15

metabolization by the organism. It also reduces sugar Scanning Electron Microscopy

availability, as shown in in lower water-soluble solids
values, a measure of starch dextrinization [32]. Extrusion caused a number of visible changes in
starch structure related to loss of granule shape, such
as gelatinization, plasticization and rupture of
intramolecular bonds. Native corn starch granules
exhibited a polyhedral shape with some surface marks,
probably due to the extraction process (Figure 5a). The
round starch granules and aggregates, which are
bonded by protein, are from the blue corn.

The extruded pellet produced using optimum

processing conditions (122 °C, 24.60% moisture)
contained no intact starch granules, probably because
Mi x (C M+C S)
0 5 10 15 20 25 30 35 Pe l l e t these either melted or plasticized due to the heat and
B rag g Diffractio n An g le (2
)
E xpa nde d
moisture of extrusion (Figure 5b). Cavities on the pellet
surface were probably formed by water evaporation at
the moment the sample exited the barrel. Interior
Figure 4: X-ray diffraction patterns for the whole blue corn pressure in the extruder barrel and matrix is higher
(CM)/corn starch (CS) mixture, extruded pellets and
expanded products. than room temperature, creating a decompression

a b

c d

Figure 5: Scanning electron micrographs (1200X) of a: whole blue corn/corn starch mixture; b: extruded pellet; c: extruded
pellet (67X) and d: microwave expanded products.
16 International Journal of Food Processing Technology, 2014, Vol. 1, No. 1 Navarro-Cortez, et al.

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Received on 24-06-2014 Accepted on 09-07-2014 Published on 28-08-2014

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