ARTICLE IN PRESS

JOURNAL OF
FOOD COMPOSITION
AND ANALYSIS
Journal of Food Composition and Analysis 19 (2006) 379–383
www.elsevier.com/locate/jfca

Short Communication

Vitamin retention in extruded food products

Nelofar Athar, Allan Hardacre, Grant Taylor, Suzanne Clark,
Rebecca Harding1, Jason McLaughlin
New Zealand Institute for Crop and Food Research Limited, Private Bag 11600, Palmerston North, New Zealand

Received 28 May 2004; received in revised form 26 July 2004; accepted 2 March 2005

Abstract

Crisp extruded snack food like products were produced from a range of cereal products using a short barrel, single screw snack
food extruder. The retention of B group vitamins during extrusion processing was compared for the different cereal grains and under
different extrusion conditions. This work showed that short barrel extruders used for snack food production retain between 44%
and 62% of the B group vitamins. This is considerably higher than the 20% retention for maize reported previously for long barrel
extruders. The stability of the vitamins was similar, with riboflavin and niacin having the highest stability. Pyridoxine was stable in
maize, but less so in oats and the maize+pea ingredients. Thiamin was the least stable during extrusion. It is concluded that short
term high-temperature cooking of extruded snacks allows the retention of higher levels of heat labile B vitamins than the longer time
and lower temperature cooking methods used in modern snack food extruders.
r 2006 Published by Elsevier Inc.

Keywords: Extrusion; Nutrient retention

1. Introduction (seconds). A wide range of thermo-mechanical and

Extrusion cooking is a relatively modern, high-
temperature, short-time processing technology that
was invented in 1940s to manufacture snack foods. This
technique has gained ground in human food and animal
feed industries world-wide, primarily for the processing
of cereal grains. The best known products are low
density foamed corn and rice breakfast and snack foods
that are widely available. Similar products made from
legumes are available in Asian countries.
Extrusion cooking, particularly in the snack food
industry, is a complex process that differs from
conventional processing by using high shear rates and
high temperatures (4150 1C) for very short periods
Corresponding author. Tel.: +64 6 351 7066/6146;
fax: +64 6 351 7050.
E-mail address: atharn@crop.cri.nz (N. Athar).
1
Present address: Fonterra Cooperative Group, Private Bag 11029,
Palmerston North, New Zealand.
thermo-chemical processes are involved, including
shear, Maillard reactions, protein denaturation and
hydrolysis. These processes result in the physical,
chemical and nutritional modification of food constitu-
ents (Harper, 1981; Linko et al., 1981; Jowitt, 1984;
Zeuthin et al., 1984).
Cereal grain products are among the most important
sources of B group vitamins in the Western diet, and for
this reason there is considerable interest in retaining the
nutritional benefits of cereals during processing. Extru-
sion processing is increasingly used to process the
ingredients in muesli bars, breakfast cereals and snack
foods, the source of a significant proportion of the cereal
grain, and hence B group vitamins, in Western diets
(Cheftel, 1986). Several studies have assessed the effects
of extrusion cooking on the retention of B group
vitamins (Cheftel, 1986; Camire et al., 1990; Killeit,
1994). During the extrusion of crispbread products
(Cheftel, 1986) at a specific mechanical energy (SME)
from 0.09 to 0.13 kWh/kg, and retention times of 0.5 to

0889-1575/$ - see front matter r 2006 Published by Elsevier Inc.

doi:10.1016/j.jfca.2005.03.004
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380 N. Athar et al. / Journal of Food Composition and Analysis 19 (2006) 379–383
1 min at 178 1C, the levels of B group vitamins
decreased. From 38% to 65% of thiamine remained,
85% of riboflavin, 80% of niacin and 71–83% of
pyridoxine. Thiamine and pyridoxine were the most
thermo-labile and levels decreased linearly with tem-
perature. Camire et al. (1990) obtained similar results,
with thiamin losses increasing with barrel temperature,
and with shear and temperature as screw speed was
increased. There was some evidence that thiamine was
more sensitive to heat than riboflavin and that riboflavin
was more sensitive to shear. Many of the studies
reported using twin-screw extruders for their ability to
operate over a wide range of conditions. However, many
of the most widely consumed expanded snack foods are
processed in short barrel, low residence time extruders,
similar to the machine used in this work.
In this paper, the retention of B group vitamins
during extrusion processing of whole oat grain and
maize and pea grits is compared for a short barrel, low
residence time extruder at different temperatures. This
information is useful for estimating the loss of im-
portant vitamins during the manufacture of extruded
snack products from a diverse range of ingredients.
2. Material and methods
2.1. Cereal ingredients
Commercially available, specification 220 maize
(corn) grits were purchased from Corson Grain Ltd
(Box 1046, Gisborne, NZ). The maize grits are
degermed before manufacture and for this reason
contain about 75% starch, about 8% protein and less
than 0.5% oil. Dried green peas (variety Rex, Crop and
Food Research) were coarsely roller milled and sieved in
our laboratory to produce a pea grit product of similar
size to the spec. 220 maize. The pea grits contained
approximately 43% starch, about 22% protein and
1.3% oil. An unmilled naked oat variety (CRO 59) was
used as the whole grain. Whole oats contain approxi-
mately 62% starch, about 11% protein and 4% oil.
They therefore contain far more oil than the other grain
products, and this is likely to alter their processing
properties. Because pea grits did not extrude well in the
equipment available due to their high protein content,
they were blended 50/50 with maize grits. In all cases the
ingredients contained about 12% moisture as used.
2.2. Extrusion processing
The food products used in this study were made on a
Dorsey, single-screw, short barrel (90 mm) snack food
extruder. The extruder was fitted with a 4-start screw
and a 2-hole die with 5 mm apertures. The ingredients
were fed into the extruder in the form of a dry granular
material at the rate of 75 g min
1 using a mass flow
feeding device. The extruder was operated at barrel
temperatures between 130 and 160 1C. No water was
added, but steam generated from the moisture in the hot
starchy melt formed from the maize and maize+pea
ingredients under high shear and temperature caused the
extrudate to expand as it left the die to form a low-
density starch-based foam. The plastic foam set rapidly
as it left the die, forming a light, crispy, rigid material
similar to many well known snack foods. During the
extrusion process, moisture was lost from the grain
products. Typically about 5% of the initial moisture is
lost, and the extrusions contain about 7% moisture. The
high oil content of the oats prevented the formation of a
well-structured foam, and this particular extrudate was
hard and dense. As the extrudate emerged from the die,
it was cut into 20–30 mm long snack-like extrusions with
a rotating knife.
Energy usage during extrusion varied between the
grits used in the experiment. For the maize and
maize+pea grits, the current drawn by the motor
driving the extruder screw was set from 12–14 A,
corresponding to a power of from 7.1 to 8.2 kW, which
in turn corresponded to a SME input of about
0.095 kWh kg
1 of ingredients. The high oil content in
the oats reduced this considerably to about
0.012 kWh kg
1 of grain. The values for the maize and
maize+pea ingredients were similar to those quoted by
Cheftel (1986) but in comparison to the 0.5–1 min
residence times used in that study, the short barrel
extruder used in this work had a residence time of
about 5 s.
2.3. B group vitamins
2.3.1. Vitamin analysis
The samples of extrudate were ground to a homo-
genous state using a food processor. Analysis of four B
group vitamins (thiamin, riboflavin, niacin and pyridox-
ine) was performed using HPLC by a commercial
analytical laboratory (AgriQuality New Zealand).
Thiamin analysis. A portion of the sample was acid
autoclaved at 121 1C, followed by enzymatic digestion to
release protein-bound vitamin and break any thiamin–
phosphate bonds. The extract was then assayed by ion-
pair reversed phase HPLC with a buffered mobile phase
(methanol–citrate, pH 2.4). The thiamin was oxidized to
thiochrome by post-column reaction with hexacyano-
ferrate (III) and detected by fluorescence (Gehring et al.,
1995).
Riboflavin analysis. A portion of the sample was acid
autoclaved at 121 1C, followed by enzymatic digestion to
release protein-bound vitamin and break any riboflavin-
phosphate bonds. The extract was assayed by reversed-
phase, ion-pair HPLC techniques and detected by
fluorescence detection (Egberg and Potter, 1975).
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N. Athar et al. / Journal of Food Composition and Analysis 19 (2006) 379–383 381

Niacin analysis. A portion of the sample was heated 3. Results and discussion
with dilute hydrochloric acid to extract the vitamin and
hydrolyze the niacinamide to niacin. The extract was Apart from the absolute values for vitamin concen-
cooled, made to a known volume and subjected to trations presented for comparison in Table 1, these data
HPLC analysis, using reversed-phase, ion-pair techni- are reported as percent retention. By comparing
ques and UV detection (Woollard, 1984). individual duplicates and the data for the maize grits
Pyridoxine analysis. A portion of the samples was across the three experiments it appears that the error
dephosphorylated by enzymatic hydrolysis for the variation in the values is about 710%. This is high but
analysis of pyridoxine. Pyridoxamine is transformed expected when low levels of vitamins are involved and
into Pyridoxal by reacting with glyoxylic acid in the may be conservative when compared with the 38–65%
presence of Fe2+, which is then reduced to pyridoxine losses of thiamin reported by Cheftel (1986).
by the action of sodium borohydride in alkaline
medium. The extract was then assayed for pyridoxine
by reversed-phase, ion-pair HPLC with fluorescence 3.1. Experiment 1: extrusion of three cereals
detection (Bitsch and Moller, 1989; Reitzer-Bergaentzle
and Marchioni, 1993). The levels of selected B group vitamins measured in
the ingredients before extrusion are shown in Table 1.
2.3.2. Vitamin retention Extrusion resulted in only slight changes in protein, fat
Samples of the cereal ingredients were analyzed for and carbohydrate levels and no changes in the levels of
vitamin content before and after extrusion. To allow for eight mineral elements (calcium, iron, magnesium,
any changes in vitamin concentration, the retention phosphorus, potassium, sodium, zinc and copper; data
factors for the products were calculated using the true not shown). However, major changes were observed in
retention method (Bergström, 1998). The equation used the levels of important B group vitamins including
for calculating true retention is thiamin and pyridoxine that are regarded as the most
heat sensitive (Cheftel, 1986). Since retinol was not
True retention ð%Þ ¼ ðVitamin content of detected in any of three cereal samples prior to
extruded cereal  g extrudateÞ= extrusion, it was decided not to analyse for retinol in
post-extrusion samples.
ðVitamin content of raw cereal
There was, of course, variation in the level of B group
 g ingredientsÞ  100: vitamins between the cereal ingredients with the maize
grits having the lowest overall vitamin content and the
2.3.3. Experiments maize+pea grits mixture having the highest levels.
Three experiments were performed. In the first, the The retention of thiamin, riboflavin, niacin and
vitamin retention of extrusions made from maize grits, a pyridoxine varied depending on the cereal type
50/50 mixture of maize+pea grits, and whole oat were (Table 2). Overall, the retention of riboflavin and niacin
compared during extrusion at 152 1C. In the second was highest, with the exception of 100% retention of
experiment, the effect of barrel temperature on the
retention of vitamins during the extrusion of maize grits
Table 1
was compared. For the third experiment, extrusion was
Vitamin levels in the cereals before extrusion
carried out at a barrel temperature of 160 1C and maize
germ material and/or amylose starch were added to Vitamins (mg/100 g) Oats Maize Maize+peas
maize grits. The germ material was added to increase
Thiamin 0.11 0.09 0.22
natural levels of the B group vitamins. Amylose starch Riboflavin 0.06 0.04 0.08
was added to increase the levels of slowly digestible fibre Niacin 1.35 0.63 1.85
in possible snack products. Four formulations were Pyridoxine 0.10 0.04 0.06
used: 100% maize, 90% maize with 10% germ material,
80% maize with 20% amylose starch added, and finally
70% maize, 20% amylose, and 10% germ material.
For each formulation and temperature, three repli- Table 2
cates of each material were produced. However for cost Vitamin retention (% retained) for B group vitamins after extrusion
reasons, the three replicates were pooled and two sub- Vitamins (% retained) Oats Maize Maize+peas
samples of each extrusion analysed for B group
vitamins. Statistical analysis of the results was not Thiamin 23 44 61
therefore possible. However, similar materials were Riboflavin 100 86 70
Niacin 100 75 60
measured in each of the three experiments and this can Pyridoxine 35 100 18
be used to gauge the consistency of the data presented.
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382 N. Athar et al. / Journal of Food Composition and Analysis 19 (2006) 379–383

pyridoxine in maize. Retention was poorest for Table 3

Vitamin retention for B group vitamins at different extrusion
thiamin and for pyridoxine in the oats and maize+pea
temperatures
extrusions.
The retention of vitamins in each cereal during the Vitamins (% retained) 130 1C 140 1C 150 1C 160 1C
extrusion process did not appear to be related to initial
Thiamin 62 62 67 62
levels of the vitamins; for example, the maize+pea
Riboflavin 100 100 67 100
mixture had the lowest retention of niacin, yet the Niacin 83 69 64 73
highest absolute level of niacin before extrusion. Pyridoxine 86 86 67 100
Differences between the oats, maize and maize+pea
ingredients are interesting because of the large differ-
ences in the SME applied to these two groups.
Surprisingly, the low SME applied to the oats during Table 4
extrusion resulted in very low retention of thiamin and Vitamin retention of B group vitamins in extruded maize with
additives of maize germ material and/or amylose starch
pyridoxine compared to maize alone. A similar low
value was obtained for the maize+pea mixture also. Vitamins 100% 90% maize, 80% maize, 70% maize,
This suggests that thiamin and pyridoxine in oats and (% retained) maize 10% germ 20% 20% amylose,
pyridoxine in peas may be more labile during extrusion amylose 10% germ
than in maize. One of the duplicate pre-extrusion Thiamin 79 86 83 70
samples used to determine the retention of thiamin after Riboflavin 100 100 100 82
extrusion for the maize sample had a value much higher Niacin 90 86 100 94
than similar values obtained from experiments 2 and 3. Pyridoxine 78 74 74 92
Ignoring this value would return a thiamin retention
value of 50%, much closer to the 62–79% obtained in
experiments 2 and 3.
the loss of B vitamins was independent of temperature
3.2. Experiment 2: effect of extrusion temperature (Table 3).

Maize grits did not expand fully during extrusion at
temperatures below 130 1C and some grits remained
intact in the extruded product, whereas the extrudates
were overcooked and unacceptably brown in colour at
barrel temperatures greater than 160 1C. Hence, the
experiments were carried out at temperatures of 130,
140, 150, and 160 1C.
This temperature range had little differential effect on
the retention of any of the vitamins. Thiamin and
pyridoxine, reported earlier to be the most thermo-
sensitive, decreased during extrusion along with niacin.
However, they decreased by the same amount at all
temperatures. In contrast, other studies (Beetner et al.,
1974, 1976; Harper, 1979; Camire et al., 1990; Killeit,
1994) have shown that the percentage of thiamine
retained decreased from 40% to 60% to between 50%
and 20% as temperatures increased from 140 to 190 1C.
These data represent a huge range in variation and
suggest that variables other than temperature may play
a role. One study (Björck and Asp, 1983) found that an
increase in barrel temperature increases riboflavin
retention possibly due to a decrease in shear resulting
from decreases in melt viscosity at higher temperatures.
In contrast with the study, other researchers did not
use a low residence time extruder. Killeit (1994) noted
that increasing throughput, and therefore decreasing
residence times, improved the retention of the B
vitamins. Our work supports this and suggests that over
the useful temperature operating range of this extruder,
3.3. Experiment 3: vitamin retention in maize with
different additives
The addition of maize germ material and amylose
starch to maize, either separately or together, did not
affect vitamin retention in the extrudates nor did the
addition of the germ material increase the levels of
thiamin in the extrudate. In effect, the results for the
additives experiment were similar to those of the
temperature experiment and the results for maize only
in experiment 1 (Table 4).
4. Conclusion
This work showed that for low retention times in a
short barrel extruder, the retention of B group vitamins
was unaffected by temperature and other ingredients.
This provides evidence that the short barrel extruders
used for snack food production retain a reasonably high
level of the B group vitamins. Compared with other
published work that used long barrel extruders with
high retention times and found only 20% retention of
the heat labile thiamin in maize extrudates, thiamin
retention in the maize extrudates in this work was not
less than 62% for experiments 2 and 3 and 44% in
experiment 1. Pyridoxine is also regarded as heat labile.
However, there was little evidence of this for maize grits
(Experiments 1 and 2).
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N. Athar et al. / Journal of Food Composition and Analysis 19 (2006) 379–383
Overall, trends for the stability of the vitamins were
similar, with riboflavin and niacin having the highest
stability. Pyridoxine was stable in maize but less so in
oats and the maize+pea ingredient. Overall, thiamin
showed the greatest reductions during extrusion.
It was not evident what the mechanism for reduction
of vitamins was. Clearly, heat labiality was at least in
part related to the grain variety used. Equally it is clear
that the extrusion process had an effect. However,
increasing the temperature of the extrudate did not
increase the loss of vitamins. It is, therefore, suggested
that there may be initial loss of a less stable fraction and
that the vitamin component retained may be a more
stable or protected form.
Recommendation
Based on the indicative results of these exploratory
experiments, we plan to re-run similar experiments with
more replicates.
References
Beetner, G., Tsao, T., Frey, A., Harper, J., 1974. Degradation of
thiamin and riboflavin during extrusion processing. Journal of
Food Science 39, 207–208.
Beetner, G., Tsao, T., Frey, A., Lorenz, K., 1976. Stability of thiamin
and riboflavin during extrusion processing of triticale. Journal of
Milk and Food Technology 39, 244–245.
Bergström, L., 1998. Nutrient Losses and Gains in the Preparation of
Food. Livsmedelsverket, National Food Administration, Sweden.
383
Bitsch, R., Moller, J., 1989. Analysis of PYRIDOXINE vitamers in
foods using a modified high-performance liquid chromatographic
method. Journal of Chromatography 463 (1), 207–221.
Björck, I., Asp, N.-G., 1983. The effects of extrusion-cooking on
nutritional value. A literature review. Journal of Food Engineering
2, 281–308.
Camire, M.E., Camire, A., Krumhar, K., 1990. Chemical and
nutritional changes in foods during extrusion. Critical Reviews in
Food Science and Nutrition 29, 35–57.
Cheftel, J.C., 1986. Nutritional effects of extrusion cooking. Food
Chemistry 20, 263–283.
Egberg, D.C., Potter, R.H., 1975. An improved automated determina-
tion of riboflavine in food products. Journal of Agricultural and
Food Chemistry 23, 815–820.
Gehring, T.A., Cooper, W.M., Holder, C.L., Thomson, H.C., 1995.
Liquid chromatographic determination of thiamin in rodent feed
by postcolumn derivatization and fluorescence detection. Journal
of AOAC International 78, 307–309.
Harper, J.M., 1979. Food extrusion. Critical Reviews in Food Science
and Nutrition 11, 155.
Harper, J.M., 1981. Extrusion of foods, vols. 1 and 2. CRC Press,
Boca Raton, FL.
Jowitt, R. (Ed.), 1984. Extrusion-cooking Technology. Elsevier
Applied Science Publishers, London.
Killeit, U., 1994. Vitamin retention in extrusion cooking. Food
Chemsitry, 149–155.
Linko, P., Colonna, P., Mercier, C., 1981. High temperature, short
time extrusion-cooking. Advances in Cereal Science and Technol-
ogy 4, 145–235.
Reitzer-Bergaentzle, A., Marchioni, M., 1993. HPLC determination of
vitamin PYRIDOXINE in foods. Food Chemistry 48, 321–324.
Woollard, D.C., 1984. New ion-pair reagent for the HPLC separation
of B-group vitamins in pharmaceuticals. Journal of Chromato-
graphy 301, 470–476.
Zeuthin, P., Cheftel, J.C., Eriksson, C., Jul, M., Leniger, H., Linko, P.,
Varela, G., Vos, G. (Eds.), 1984. Thermal processing and quality of
foods. Elsevier Applied Science Publishers, London.