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Corresponding author. ABSTRACT
TEL: +91-98599-11865;
FAX: +91-03661-277143; Today, fried foods are very famous everywhere around the world and it can be
EMAIL: pk.nayak@cit.ac.in observed by the increasing number of fast food restaurants in the last few decades.
Deep frying of foods at high temperature enhances the sensorial properties which
Received for Publication April 19, 2015 include the unique fried flavor, golden brown color and crispy texture. Chemical
Accepted for Publication October 1, 2015
reactions like oxidation, polymerization, hydrolysis, etc., take place in the food
system, which ultimately alters the physical and chemical properties of fat. Conse-
doi:10.1111/jfbc.12215
quently, so many by-products such as free fatty acids, alcohols, cyclic compounds,
dimers and polymers are produced. Therefore, it is necessary to understand the
physical and chemical changes during deep fat frying to monitor the quality of
fried foods. In this review, we constituted the previous studies on the changes in
fats during frying and methods used to analyze the quality of fried oil, in order to
explore the areas which require further research.
PRACTICAL APPLICATIONS
Deep frying is the most common and one of the oldest methods of food prepara-
tion worldwide. To reduce the expenses, the oil tends to be used repeatedly for
frying. Repeated use of this oil has become a common practice due to low level of
awareness among the public about the bad effect of this practice. Nowadays, the
consumption of deep-fried food has gained popularity which may cause increased
risk of obesity. When heated repeatedly, changes in physical appearance of the oil
will occur such as increased viscosity and darkening in color, which may alter the
fatty acid composition of the oil. In this review, we have investigated the detail
mechanism of decay of oil and parameters to be measured to know the quality
and safety of oil.
TABLE 1. QUALITY PARAMETERS OF COOKING OIL oil complement, fryer model and use of filters (Lalas et al.
FFA Viscosity 2006; Mariana et al. 2014). Different factors such as fatty
(Acid PV IV (mPA s) Saponification acid composition of oil, product quality, frying time, tem-
Oil Type Value) (meq./kg) (g/100g) at 400C Value perature, heating type, composition of frying oil, composi-
Soybean 1.15 10 139 33 195 tion of fried food, fryer type, antioxidants and oxygen
Sunflower 1.21 6.6 134 35 193 availability affect the deprivation of oil.
Mustard 1.5 20 125 48 184 Several studies have been carried out on degradation of
Palm 1.75 3.18 45 29 202 oil, but a systematic study and the effect of oil deterioration
Olive 6.6 10 94 40 196
have not been studied yet. This review is an approach
towards the investigation of the detail mechanism of decay
of oil and parameters to be measured to determine the
quality index of oil.
further cooking purposes without discarding it. Azman
et al. (2012) have determined the level of knowledge, atti-
tude and practice of night market food outlet operators in Phenomenon Responsible for Quality
Kuala Lumpur, Malaysia regarding the usage of repeatedly Changes during Deep Fat Frying
heated cooking oil. They have collected data from the
Phenomenal changes involve increase in the concentration
respondents (n = 100) by face-to-face interview and
of free fatty acids, as well as polar materials, polymeric com-
observed that majority of respondents had only moderate
pounds and decrease in the unsaturated fatty acid composi-
(53.0%) or low (18.0%) level of knowledge regarding this
tion. (Kassama 2003). It mainly depends on three types of
issue. Most respondents (67.0%) agreed that it is not a
chemical reactions such as hydrolysis, oxidation and polym-
good practice. The majority (69.0%) agreed that the usage
erization. Oil becomes more stable if it contains lower levels
of repeatedly heated cooking oil is detrimental to health.
of linoleic, linolenic acid and higher levels of oleic acid
Despite that, most respondents (63.0%) admitted that they
(Aladedunye and Przybylski 2013). Decomposition of
had used cooking oil repeatedly. Most (62.0%) of the
linolic acid produces 2,4-decadienal which is responsible for
cooking oil samples taken from the night market food
deep-fried flavor.
outlets were considered fit for human consumption.
Saxena 2014 conducted a study jointly with the National
Diabetes, Obesity and Cholesterol (N-DOC) Foundation,
IIT-Delhi and Diabetes Foundation of India (DFI) that has Hydrolysis
revealed that reuse of oil in home-cooked food forms a It involves the breakage of triglycerides in the presence
heavy dose of trans-fatty acids (TFA). A random sample of water and steam (Coultate 1989). It produces
survey of 402 women between the age group of 25 and 60 monoglycerides, diglycerides, free fatty acids and glycerol,
across Delhi was conducted by a team of researchers to eventually (Fig. 1). The extent of hydrolysis depends on the
monitor the pattern of usage of oil while cooking. Besides oil temperature, interface area between oil and the aqueous
highlighting the harmful effects of TFA, the study has also phase, amounts of water and steam. Free fatty acids and
raised some serious concern over the cooking practice in lower molecular weight acidic products arising from fat oxi-
many households. Nearly 43.3% of the women reuse the fat dation enhance the hydrolysis process in presence of steam
or oil (used for frying) at least two to three times for
cooking. Also, 54% of the women left the used oil after
frying in the same utensil in which the frying was done, and
merely 6% of women drained off the used oil before
storing.
This imparts negative effects on the health condition of
consumers. The process of oxidation in the human body is
assumed to be a causal factor of certain diseases such as car-
diovascular, cancer, early aging, or cataract. Furthermore,
discarding the deteriorated oil to the environment enhances
pollution.
The presence of air and water further accelerates the dete-
rioration of frying oil (Chatzilazarou et al. 2006). It also FIG. 1. FORMATION OF FATTY ACIDS AND DIACYL GLYCEROLS
depends on the nature of the fried material, the frying oil, (AOCS LIPID LIBRARY, OILS & FATS, FORMATION OF NEW
time, temperature, intermittent continuous heating, fresh COMPOUNDS DURING FRYING – GENERAL OBSERVATIONS, 2009)
during frying (Pokorny 1989). The extent of hydrolysis can lyze the reactions while the formation and decomposition of
be determined by the saponification value of oil. peroxide radical takes place in a reversible way.
Termination involves the formation of final products like
nonpolar dimer, oxidized monomer, oligomer, alcohols,
Oxidation aldehydes, ketones, acids, lactones, etc. Silvagni et al. 2010
Three types of oxidation take place in deep-fried oil such as have explained formation of aldehyde directly from peroxyl
autoxidation, thermal oxidation and photosensitized oxida- radical through an independent pathway during the thermal
tion. The oxidation by direct combination with oxygen at treatment of peanut oil at 180C and it can be qualitatively
ordinary temperature is called autoxidation. It results in the analyzed by gas chromatography (Marmesat et al. 2008).
rancidity of oil, which causes unpalatable odor and flavor Frying temperature, the number of frying process, the con-
due to the oxidative or hydrolytic degradation of oil. tents of free fatty acids, polyvalent metals and unsaturated
(Shukla and Bhattacharya 2004). Oxidative rancidity fatty acids of oil decreases the oxidative stability and flavor
involves oxygen attack of glycerides and occurs in all kinds quality of oil. While antioxidants play an important role in
of unsaturated fats (Sangle and Daptare 2014). Thermal decreasing the frying oil oxidation, the effectiveness of anti-
oxidation occurs due to heating at high temperature more oxidant decreases with elevated frying temperature.
than 180C (Marinova et al. 2012). The rate of thermal oxi- Oxidation is one of the most important deteriorative
dation is faster than the autoxidation (Choe and Min 2007). changes that occur in deep-fried oil and it comprises of five
All the above said oxidation processes follow a mechanism main stages, namely induction period, peroxide formation,
known as free radical mechanism (Fig. 2). It mainly involves peroxide decomposition, polymerization and degradation,
three steps: chain initiation, propagation and termination. as shown in Fig. 3.
In chain initiation, the reactions goi ahead by heat, light Photo-oxidation occurs when normal triplet oxygen are
and metal catalyst with the formation of alkyl free radical converted to a singlet oxygen by the exposure of ultraviolet
(R) (Halliwell and Gutteridge 1984). (UV) radiation. The singlet oxygen interacts with polyun-
In propagation, the radical formed in the first step reacts saturated fatty acids to form hydroxyl peroxide which initi-
with oxygen to form the peroxy radical (ROO) (Halliwell ate the autoxidation reaction.
and Gutteridge 1984). The levels of peroxy radicals are
Change in Physical Parameters during Deep
higher than lipid free radicals. Peroxy radical abstracts
Fat Frying
hydrogen from another lipid molecule and forms lipid
radical (R + ROOH). The hydroperoxides are very unstable Physical changes in oil due to deep fat frying include
and gives rise to short chain compounds by the cleavage of increase in color, foaming and viscosity. There are various
O-O, C-C and C-O bonds around the peroxide group to methods to measure these changes. The qualitative changes
decompose into short chain compounds. The radicals cata- can be evaluated by visual inspection.
heating of oil, reactions like oxidation, polymerization, The different arrangement of fatty acids on glycerol back-
isomerization (in both frying and heating) and hydrolysis bone of tri-glyceride molecules changes the viscosity of oil.
(in frying) occur; as a result, several polymers were gener- Zahir et al. (2014) have studied that at 35C viscosity of
ated. The change in palm oil density is more than olive oil, mustard oil is higher than corn oil due to the degree of
suggesting that the generation of higher polymer content in unsaturation of oil. Sharova and Ramadan (2012) have
palm oil than olive oil and change in the density was more investigated the effect of unsaturation upon the viscosity of
pronounced after the 20th cycle of frying. sunflower oil (SO), cottonseed oil (CO) and palm oil (PO)
Zahir et al. (2014) have observed that the density of and found that the major fatty acids C18:1 and C18:2
corn and mustard oil were decreased with the rise in tem- appeared to make a great contribution towards the flowing
perature as well as with using the same oil for frying of behavior. The viscosity of oil increases with the increase in
potato for three times. The densities of oil were related to the level of C18:2 and decreases the level of C18:1 fatty acids
the standard value in the range of 0.898–0.907 g/mL (Fig. 5 – relation between the levels of C18:2 and viscosity
(SON, Standard Organization of Nigeria, 2000).They also in different oil and Fig. 6 – relation between the levels of
observed the density values of 0.9694 and 0.9223 g/mL for C18:1 and viscosity in different oil).
mustard and corn oil, respectively, at room temperature The presence of double bond does not allow fatty acid
(35C). It may be due to the pi bonds which make the more molecules to stay closely together; therefore, they will inter-
rigid bonds and the more strenuous rotation between C-C fere with packing in the crystalline state (Abramovic and
bonds. Klofutar 1998; Aravindan et al. 2007). Thus, fatty acids with
higher number of double bonds will not be rigid and
behave like fluids when they are packed loosely (Kim et al.
Viscosity
2010).
Viscosity is one of the indicators used to evaluate the physi- Viscosity is strongly affected when exposed to higher
cal changes in edible oil. It depends upon density, molecular temperatures, air and increase in the number of frying
weight, melting point, degree of unsaturation and tempera- cycles, and it enhances the formation of oxidative and poly-
ture (Sharova and Ramadan 2012).Viscosity increases meric compounds and increases the tendency to foam
during hydrogenation as the increase in the chain length of during frying (Samah and Fyka 2002). Tarmizi et al. (2013)
tri-glyceride fatty acid and decreases during unsaturation of have studied that the viscosity of oil increased significantly
fatty acids (Santos et al. 2004). Further polymerization of in the case of vacuum and atmospheric drainage after 2 days
oil and formation of dimmer, polymer products with of frying from 45.48 to 54.12 and 55.97 mPa·s, respectively
molecular weight between 690 and 1,600 Da increases the (Fig. 7). After 80 batches of frying, polar compounds
viscosity of oil (Choe and Min 2007). Oil rich in linoleic increased from 7.81 to 15.03% and 17.19 % in the case of
acid are more easily polymerized during deep fat frying vacuum drainage and atmospheric drainage, respectively.
than the oil rich in oleic acid (Formo et al. 1979; Takeoka This is due to the formation of higher molecular weight
et al. 1997; Valdes and Garcia 2006). Santos et al. (2005) polymeric compounds upon increase in frying time.
have observed that heating of oil (190C) for several hours The similar effect was observed by Debnath et al. (2012).
will not change the Newtonian behavior of several types of They observed the kinematic viscosity of rice bran oil as
oil including olive. 3.39 × 10−6 m2/s. This value was increased by increasing the
number of consecutive frying cycles (Lalas et al. 2006). Vis- from 30 to 180C. When temperature increases, the viscosity
cosity of oil also depends upon the measuring temperature. of oil decreases as a result of increase in kinetic energy,
Lioumbas et al. (2012) have determined the viscosity of which enhances the movement of molecules and reduces
olive oil and palm oil by varying the measuring temperature the intermolecular forces.
TABLE 2. COMPOSITION OF LONG CHAIN FATTY ACIDS IN EDIBLE OIL SAMPLES (MISTRY AND MIN 1992)
frying temperatures. The value decreased about 6.3, temperature in the presence of moisture and air forms FFA.
9.72 and 26.52% during frying at 150, 200 and 250C, In particular, it is damaging to the stability of the frying
respectively. medium and the fried foods. These are rapidly oxidized, and
they catalyze further oxidation of polyunsaturated fats by
solubilization and activation of catalytic metal salts. Their
Iodine Value
surface activity increases their contact with oxidizable com-
The iodine value (IV) of oil is a direct representation of the ponents of the food, and promotes lipid protein interac-
degree of unsaturation of the oil. Iodine is used to haloge- tions (Urbancic et al. 2014). The maximum allowed value of
nate the double bonds present in unsaturated fatty acids. FFA varies depending on the type of food being fried and
The IV is expressed in the number of centigrams of iodine number of batches during frying operation (Shaker 2014).
absorbed (Rangana 2005). The research carried out by Gunstone (2008) suggested that the FFA content of the
Abdulkarim et al. (2005) showed the changes in IV during refined oil should be less than 0.1% because most of the
5 days of frying and the changes in the IV values from FFAs from crude oil are removed during the refining
day 0 to day 5were recorded as follows: canola oil (CO) process. Casal et al. (2010) found out that the acidity of the
(109.9–103.0), soybean oil (SO) (116.9–111.8), palm oil commercial olive oil was higher than virgin olive oil and
(PO) (56.8–53.7) and Moringa oleifera oil (MO) (65.9– they observed that it may be due to the removal of free fatty
62.2). The change in the IV values for the above said oil was acid during saponification. Sebastian et al. (2014) have
in the order of CO > SO>PO > MO. MO and PO had a found that the FFA levels in fresh oil samples varied from
longer induction period since there were no significant 0.05 to 0.08% and, for in-use samples from the fryer, ranged
changes for the first two days of frying. In canola oil and widely from 0.25 to 3.99%. For the industrial production of
soybean oil, the changes in the IV were significant after the potato chips, the FFA level of 0.5% has been reported as the
first day of frying, indicating shorter induction periods. threshold for discarding the used frying oil, whereas a
This was largely due to the high amounts of linolenic acid maximum value of 1% FFA is usually allowed by the proces-
present in the two samples of oil (Abdulkarim et al. 2005). sors of pre-fried French fries (Ismail 2005). Higher FFA
Pineda et al. (2011) have observed a steady decrease in concentrations are tolerated in the case of oil used for frying
the IV of sunflower oil, olive oil and high oleic acid sun- battered and breaded products (2–2.5%) (Tarmizi et al.
flower oil (HOSO) during frying. It may be due to the 2013).
decrease in the unsaturation of the oil samples. Frying leads The FFA value increases with time of frying (Naz et al.
to decrease in the unsaturation for all types of oil; this de- 2005) as shown in Fig. 9 – effect of deep frying on FFA
crease in IV is a result of complex physio-chemical changes levels of olive, corn and soybean oil. Furthermore, this value
and indicates the decrease in oxidation rate (Lalas 2009). changes with the variation of food product. They observed
IVs of all the oil samples exposed to air and air–light did that the FFA of chicken drum sticks was higher than that of
not change significantly, whereas deep frying substantially the oil used for deep frying of French fries (Fig. 10).
reduce the IVs (Naz et al. 2005). Oxidation, which consists Though, the moisture in potato (76.7%) is more than in
of a complex series of chemical reactions, is characterized chicken (70%), and the thermal conductivity of both food-
by a decrease in the total unsaturated content of the oil due stuffs are almost the same (0.54 W/(m.K)), the FFA of corn
to abstraction of hydrogen adjacent to the double bond and oil used for frying of chicken was slightly greater as com-
the formation of free radicals. Hence, deep frying that accel- pared to FFA of the oil used for potato. It is due to the fatty
erates the oxidation of the oil causes maximum reduction of acids released from fat-containing foods such as chicken
the IVs. However, no significant differences were found in and their concentration in the frying oil increases with con-
case of deep frying with respect to frying time. tinuous use.
FFA value increases with increase in the number of frying
cycles and heating. The change in FFA after frying is more
Free Fatty Acids/Acid Value
in comparison to heating. The increase in FFA is because of
Free fatty acids (FFA) value is the number of milligrams of the cleavage and the oxidation of double bonds to form car-
KOH required to neutralize the free fatty acids present in bonyl compounds and low molecular fatty acids during
1 g of oil. If the free fatty acid content of coconut oil or frying. The moisture coming from fried products accelerates
palm oil has to be in the percentage of weight, the calcula- the hydrolysis and it is due to fact that water can promote
tion is based on the molecular weight of lauric acid. the hydrolysis of triacylglycerol to form combination of
(Rangana 2005). mono and diacyl glycerol, glycerol and free fatty acids.
This is a fast, reliable method to monitor the acidity of oil Debnath et al. (2012) have found that the FFA value of rice
during frying (Bensmira et al. 2007). The hydrolysis of tri- bran oil increases from 0.3 to 0.44% and 0.48 % after
glycerides and decomposition of hydroperoxide at high heating and frying for one to six consecutives cycles, respec-
tively. The increase in FFA value is not an unswerving (Atinafu and Bodemo 2011). In determination of this value,
parameter for degradation of frying oil because it is difficult the hydroperoxides reacts with acidified potassium iodide to
to differentiate between FFA formed by oxidation or by liberate iodine that can be measured volumetrically by reac-
hydrolysis (Frega et al. 1999; Mohamed et al. 2006). FFA tion with standardized sodium thiosulphate. The value rep-
value is independent of the levels of linoleic acid and resents milli equivalent of oxygen per kg of fat. Cheman and
tocopherol (Aladedunye and Przybylski 2013). Wanhussin (1998) mentioned that a good-quality vegetable
oil should have a PV of lower than 2 meq/kg. A decrease in
PV during frying has been observed by several researchers
Peroxide Value
(White 1991; Vieira and Regitano-D’arce 1999; Zhang et al.
Peroxide value (PV) is a useful indicator of oxidation at the 2007). The primary product of lipid oxidation is hydroper-
initial stage, but it is not related to the frying duration oxide, which is generally referred to as peroxides (Allendorf
2010). PV is influenced by constituent fatty acids and the
length or type of storage (Lawson 1995).
PV may increase after the sample is taken from the fryer.
Therefore, PV is generally not a very reliable parameter to
determine deterioration of cooking oil (Man and Hussain
1998). Marinova et al. (2012) have investigated the effect of
heating at 180C on the PV of oil samples (Fig. 11) and they
found out that the PV was not a representative for the
changes occurring in the oil samples, and storage of oil only
leads to increase in PV. The use of oil for frying does not
lead to substantial increases in PV because peroxides
decompose spontaneously above 150C (Marmesat et al.
2010). Chen et al. (2014) have correlated PV of palm oil
with frying temperature. The highest value was found at
150C, followed by significant decrease at 200C and slight
increase at 250C. This can be explained by the thermal
decomposition of hydroperoxides to carbonyl and aldehyde
compounds during deep fat frying at higher temperature,
which results in lower accumulation in the oil at higher
frying temperature.
Pineda et al. (2011) have observed that at 160C, PVs
FIG. 10. VARIATION IN FFA LEVELS DUE TO VARIATION IN NATURE OF showed a slight increase during the first 20 frying cycles fol-
FRIED FOOD (NAZ ET AL. 2005) lowed by a decrease in PV. At 180C, PVs showed a slight
increase at 10 cycles, remaining almost constant after 15 reagent, according to the International Union of Pure and
frying cycles. At a higher temperature (180C), PVs are lower Applied Chemistry method (Paquat and Hautfenne 1987).
at severe frying conditions as peroxide decomposition rate It is also defined as the relative amount of nonvolatile
becomes higher than peroxide formation rate. As peroxides unsaturated aldehyde compounds formed by the secondary
are transient chemical compounds, they are also unstable degradation products from fatty acid hydroperoxide. List
under frying conditions. There is equilibrium between per- et al. (1974) were the first researchers to use the p-AV test to
oxide formation rate and peroxide degradation rate and judge oil quality and had demonstrated a highly significant
similar behavior was observed by Casal et al. (2010) for linear correlation (r = −0.82) between p-AV and flavor
olive oil. scores in soybean salad oil.
PV depends upon the method of heat treatment of oil. Al-Kahtani (1991) reported that the p-AV was the most
Chu and Hsu (2001) have observed that PV of gas-treated reliable measure of oil oxidation and the discarding oil has
oil was 33% higher than microwave-treated oil for frying of PV levels in the ranges 14.2 to 55.8. According to Gupta
shallot, which indicated that the quick evaporation of water (2005) a desirable p-AV for fresh frying oil should be less
by frying of shallot pieces with microwave heating produced than 4.0, with an upper limit of 6.0. He also mentioned that
less oxidized oil. if the fresh oil had a p-AV above 6, the oil would be highly
Naz et al. (2005) have suggested that the increase in PV oxidized. The secondary products of oxidation are more
of oil follows the order deep frying > air–light expo- stable than the unstable peroxides formed in the primary
sure > air exposure. Debnath et al. (2012) have determined stages of the oxidation. It increases with the increase in
the PV of fresh rice bran oil was 1.63 meqO2/kg. After frying time and levels up after the equilibration of the
heating and frying for one to six cycles, the PV was found formed carbonyl compounds with their degraded portions
to be increased from 2.2 to 3.6 meq/kg and 3 to and the transfer of these components into fried food
4 meqO2/kg respectively. For heating and frying they also (Aladedunye and Przybylski 2009). The p-AV value
concluded that oil degrade more during frying as com- decreases with the increase in tocopherol content. p-AV of
pared to heating. HOSO 4.3 (high oleic sun flower oil containing 4.3 linoleic
acid) containing higher amount of γ and δ tocopherol
isomers was lower than in HOSO 4.5 (high oleic sun flower
P-Anisidine Value
oil containing 4.3 linoleic acid) (Ali et al. 2013; Shaker
p-Anisidine value (p-AV) is defined as 100 times the optical 2014).
density measured at 350 nm in a 1 cm cell of solution con- Aladedunye and Przybylski (2013) conducted a series of
taining 1 g of oil and 100 mL of a mixture of solvent and frying trials and found that the p-AV level stabilized at 10
FIG. 13. RELATIONSHIP BETWEEN SPECIFIC EXTINCTION K232 AND THE FRYING DURING FOR SO AND MO (NZIKOU ET AL. 2009)
at lower temperatures (58C). Most of the common methods Figure 16 shows the FTIR spectra of olive oil, corn, sun-
for monitoring autoxidation and determining the oxidative flower and soybean oil samples. The fingerprint region,
stability of edible oil use elevated temperatures (above 98C) especially 1,300–1,000 cm−1, shows differences in the peak
to accelerate the oxidation process, which often changes the areas and peak heights of the absorption bands at
mechanism of oxidation and makes it difficult to extrapo- 1,163 cm−1 (assigned to -C-O stretching and CH bending)
late the data to ambient storage conditions. From different and at 1,118 and 1,097 cm−1 (assigned to -C-O stretching).
oil samples, Russin and Sedman (2004) looked at the peak
height of the peroxide (ROOH) absorption band at
Nuclear Magnetic Resonance
3,444 cm−1. The oxidation process was allowed to continue
until peroxide values were above 300 meq oxygen/kg oil. He Nuclear magnetic resonance (NMR) spectroscopy has
found that the hydroperoxide absorption band starts at played an ever-increasing role in the study of properties of
3,444 cm−1 in the spectra of oil with low PVs, but shifts to oil of vegetable origin (Soon 1984, 1985; Mallet et al. 1990;
progressively lower wave numbers as oxidation proceeds. Howarth and Vlahov 1996) during the last 10 years. The
molar percentages of unsaturated fatty acids in triglycerides shifts varying between 7.2 and 10.4 ppm where signals of
can be measured by comparing the peak areas of the allylic carbonyl group may appear, indicated clear differences
methylenes with those of the methyl signals. The volatile between heated oil samples and unused ones (Fig. 17). In
compounds of virgin olive oil have been studied by high addition, comparison done between samples A and D at
field (600 MHz) NMR spectroscopy (Sacchi et al. 1989). chemical shifts of 5.6–8.4 ppm also indicated new signals in
Muhizi et al. (2009) have carried out the NMR study of sample D. Zoomed zones showed new signals from all over
four samples of oil (sample A: staring oil, B: oil used for one heated and reused oil (samples B, C and D).
time, C: oil used for five times, D: oil used for 10 times). It
has been obtained that the signal at 2.75 ppm (zone H) was
absent from sample D, suggesting the breakdown of double Differential Scanning Calorimetry (DSC)
bonds of linoleic acid, leading to the formation of other It is used to analyze the melting property of oil. Nzikou
products. Further analysis of 1 H NMR spectra, at chemical et al. (2009) have examined the DSC (differential scanning
calorimetry) analysis of soybean oil (SO) sample before and
after 1 h of frying. The heating profile using scan rate (10C/
min) showed two major peaks at −22.54C (SOa before used)
and −23.72C (SOb after used) which were due to polyun-
saturated fatty acids and two small peaks at −5.97C (SOa)
and +2.89C (SOb), which were due to monounsaturated
fatty acids. It should be noted that the thermal behavior of
oil was not significantly affected by frying (Fig. 18).
FIG. 17. H NMR DIFFERENCE BETWEEN UNUSED OIL AND OVERHEATED AND REUSED OIL SAMPLES (RUSSIN AND SEDMAN 2004)
radical scavenging activity. Sulieman et al. (2006) has oil (polar compounds) were completely dissolved in toluene
applied this technique to measure the antioxidant potential which allowed determining the antiradical performance of
of vegetable oil during frying. Fresh oil (nonpolar com- fried oil very accurately (Sulieman et al. 2006). After 16 h
pounds) and decomposition products of deteriorated dried frying, they reported that 85% of 2,2-diphenyl-1-
picrylhydrazyl radicals were quenched by palm olein while
sunflower and cottonseed oil samples were able to quench
77 and 72%, respectively. The stronger radical scavenging
activity of palm olein compared to sunflower and cotton-
seed oil may be due to the significant differences in the
composition of bioactive compounds and the diversity in
structural characteristics of potential antioxidants. All these
factors may contribute to the radical quenching efficiency of
vegetable oil.
Gas Chromatography
Chen et al. (2014) analyzed the TFA profiles in deep-frying
palm oil and chicken fillets with an improved gas chroma-
tography (Gc) method. The oil was heated to 150, 200 and
250C, and then a batch of 40 ± 5 g chicken fillets was added
and fried for 10 min as one frying cycle at each temperature.
In each day, the oil was continuously heated for 8 h with 48
frying cycles performed. After frying at three different tem-
FIG. 18. THERMO GRAMS OF DIFFERENTIAL SCANNING peratures of 150, 200 and 250C, TFAs in frying oil samples
CALORIMETRY ANALYSIS OF OIL SAMPLES SO, (A) SOA: SOYBEAN OIL were analyzed and compared. A progressive decrease in the
UNUSED AND (B): SOB: SOYBEAN OIL USED AFTER 1 H OF FRYING content of both (cis) linoleic and (cis) linolenic acids was
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conditions. Food Chem. Toxicol. 48, 2972–2979. FREGA, N., MOZZAN, M. and LERCKER, G. 1999. Effect of
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