Application of the Oxitest® method to evaluate the Oxidation stability of edible

oils at different working temperatures under accelerated conditions

Simona Pironea , Alessandro Adobatia, Sara Limbo a, Stefania Cortib
aDeFENS– Università degli Studi di Milano, Via Celoria 2 - 20133 Milan, Italy; packlab@unimi.it
bVelp Scientifica srl- Via Stazione 16 – 20865 Usmate , Italy ; inse@velp.it

INTRODUCTION
Lipid oxidation is one of the most serious problems occurring during storage of fatty foods, causing a shortage of their
shelf
shelf--life
life.. A number of accelerated methods have been developed to test the resistance of edible fats and oils to AIM
oxidation (Farhoosh et al.
al., 2008
2008)). All these accelerated methods involve the use of elevated temperatures because the
temperature.. Oxitest® reactor (Velp Scientifica, Usmate -
rate of the oxidative reaction is exponentially related to the temperature This work aimed at:
Italy) has been successfully used to measure the resistance to oxidation of raw materials and finished food food--feed 1. Discriminating the resistance to oxidation among 5 different edible oils
oils;;
without preliminary fat separation (Mora et al. 2009)). Oxitest® is based on the absolute oxygen pressure change in a
al., 2009
2. Investigating the influence of temperature, the most relevant variable taking part
closed and thermostatic chamber, assumed as the oxygen uptake by reactive substances.substances. The tests allow to obtain an
in the autoxidation reactions
reactions..
oxidation curve, characterized by an Induction Period as the time required to reach an end point of oxidation
corresponding to either a level of detectable rancidity or a sudden change in the rate of oxidation.
oxidation.

MATERIALS AND METHODS

SAMPLE PREPARATION
Five different edible oils were used for the test. Before analysis, they present a similar POV value. Oxitest® working conditions are shown in
Table 1. Each analysis was repeated four times using two different reactors. The Oxitest® response is the Induction Period (IP) expressed as TEST CONDITIONS
a “stability time” before fat oxidation; it can be calculated by a graphical method (Figure 3). I test II test III test
Temperature (°
(°C) 90 80 70
Pressure (bar) 6 6 6

Maize oil
Virgin olive oil
Peanut oil
(glass 1L)
10g of oil was distributed Gas test oxygen oxygen oxygen
(PET 1L) (PET 1L)
POV < 10 meqO2/kg POV < 10 meqO2/kg POV < 10 meqO2/kg in each sample holders of Table 1- Oxitest ® working conditions
the reaction chambers
(Figures 1 and 2)
IP: induction period
Figure 2-
2- Oxitest ®
Figure 1-
1- Reaction chambers
of Oxitest ® reactor pressure Oxidation curve

Sunflower oil (bar)

Mixed seed oil time
(PET 1L)
(PET 1L) (h:min)
POV < 10 meqO2/kg
POV < 10 meqO2/kg Figure 3-Typical oxidation curve

RESULTS AND DISCUSSION

Resistance to oxidation: Pressure changes: average values of 4 chambers at 90°C Pressure changes: average values of 4 chambers at 80°C Pressure changes: average values of 4 chambers at 70°C
discrimination among different 7 7 7
PEANUT OIL PEANUT OIL PEANUT OIL
edible oils 6
SUNFLOWER OIL
6
SUNFLOWER OIL
6
SUNFLOWER OIL
5 5 5
MAIZE OIL MAIZE OIL
Oxidation curves of the five oils, analyzed pressure (bar) MAIZE OIL
pressure (bar)

pressure (bar)

4 VIRGIN OLIVE OIL 4 VIRGIN OLIVE OIL 4

in the same conditions (90 90°°C, 6 bar of VIRGIN OLIVE OIL
MIXED SEED OIL MIXED SEED OIL
oxygen) are shown in Figure 4. Oxitest®
3 3 3 MIXED SEED OIL

2 2
has the ability to discriminate the 2

oxidation. Table 2 shows

resistance to oil oxidation. 1 1 1

different Induction Periods which depend 0 0 0

0 10 20 30 40 50 0 20 40 60 80 100 0 50 100 150 200
on the composition of the oil and its time (h) time (h) time (h)
botanical origin
origin.. For example, oxidation of Figure 4 - Oxidation curves of edible oils with Oxitest ® at 90°
90°C Figure 5 - Oxidation curves of edible oils with Oxitest ® at 80°
80°C Figure 6 - Oxidation curves of edible oils with Oxitest ® at 70°
70°C
sunflower oil is faster (IP= (IP=1010,,9h) than
virgin olive oil (IP=
(IP=22
22,,7h), characterized by
a lower antioxidant content
content..
Temperature effect on edible oils oxidation 6
PEANUT OIL SUNFLOWER OIL MAIZE OIL
10,00 MIXED SEED OIL VIRGIN OLIVE OIL
Oxitest® reactor can be used at different temperatures and oxygen pressures. To evaluate the PEANUT OIL 5
temperature effect on the Induction Period, the oils were analyzed at 90, 80, 70°C and 6 bar
coefficient of variation (%)

SUNFLOWER OIL
of oxygen pressure. The repeatability of Oxitest® reactor is estimated using the coefficient of 5,95
5,85 4 y = 11192x - 27.62
MAIZE OIL R² = 0.993
variation of Induction Period. It rarely exceeds 5% in each analysis (Figure 7). Oxidation 5,43 5,10
y = 11169x - 27.70
ln (IP)

5,00 4,52 3
4,29 MIXED SEED OIL R² = 0.999
curves of oils are shown in Figures 4, 5, 6. They show that the trend of oil oxidation is 3,82 3,66
3,01
y = 11019x - 27.63
3,00 VIRGIN OLIVE OIL 2 R² = 0.993
the same for the three temperatures but the Induction Period increases with the decrease of 1,96
2,54
y = 11076x - 27.94
the temperature (Table 3). In particular, the relationship between IP and temperature is 0,64 0,80
1 R² = 1.00
y = 10910x - 27.62
exponential and it follows the Arrhenius law, as shown in Figure 8. Coefficients of 0,00
0,00
0
R² = 0.999

70 80 90
determination are always higher than 0.99, emphasizing a good relationship between IP Temperature (°C)
0,00270 0,00275 0,00280 0,00285
1/T (K-1)
0,00290 0,00295

and the temperature. Figure 7 - Reproducibility of oxidative oil stability expressed as coefficient of Figure 8 - Arrhenius plot for the different edible oils
variation for n=4

P T Average IP IP90 IP80 IP70 RATIO

Units (bar) (°C) (h) Units (h) (h) (h) IP90/IP70

Sunflower oil 6 90 10,9
Peanut oil 21.28 52.05 128.05 6,0
Mixed seed oil 6 90 12,6
Sunflower oil 11.46 26.17 66.08 5,8
Maize oil 6 90 14,8 Maize oil 14.52 39.04 85.47 5,9
Peanut oil 6 90 20,3 Mixed seed oil 13.08 30.78 77.46 5,9
Virgin olive oil 6 90 22,7 Virgin olive oil 23.75 64.96 143.73 6,1
Table 2 - Induction Period average values obtained with Oxitest ® Table 3 - Influence of the temperature on IP

CONCLUSION REFERENCES
With Oxitest ® reactor it is possible: 1. Comandini P., Verardo V., Maiocchi P., Carboni M.F., 2009. Accelerated oxidation: Comparative study
of a new reactor with oxidation stability instrument, in Eur. J. Lipid Sci. Technol., 111:933-940.
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to calculate the Induction Period of different edible oils and to discriminate their resistance to oil oxidation under Rancimat test conditions. European Journal of Lipid Science and Technology
oxidation; 110: 587-592.
to perform accelerated shelf-life tests, estimating the IP value at storage temperature, evaluating the 3. Mora L., Piergiovanni L., Limbo S., Maiocchi P., 2009. Valutazione della stabilità ossidativa di oli
temperature effect. vegetali mediante reattore per il test di ossidazione Oxitest ®, in Industrie Alimentari, 495.