Meat Science 66 (2004) 647657

www.elsevier.com/locate/meatsci

Study of the eects of smoke avourings on the oxidative stability

of the lipids of pork adipose tissue by means of Fourier transform
infrared spectroscopy
M.D. Guillen*, N. Cabo
Tecnologa de Alimentos, Facultad de Farmacia, UPV, Paseo de la Universidad No. 7, 01006 Vitoria, Spain
Received 22 July 2002; accepted 11 July 2003

Abstract
Pork adipose tissue was dry-salted for 24 h and then smoked by immersion in two liquid smoke avourings for 1, 2 or 3 min.
Both unsmoked and smoked pork adipose tissue samples were submitted to oxidative conditions at 70
C in a convection oven with
circulating air. Melted lipids of both samples were studied by Fourier transform infrared spectroscopy. Duplicate spectra were
collected each day of the experiment by applying a lm of melted lipids between two KBr disks. Changes in frequency values of
dierent bands and in ratios between absorbances of some bands allow oxidation degree and oxidative stability of the samples to be
determined. The usefulness of this technique for monitoring the oxidation process of pork adipose tissue lipids is shown. The
greater oxidative stability of smoked pork adipose tissue samples in comparison with unsmoked samples is proved.
# 2003 Elsevier Ltd. All rights reserved.
Keywords: Pork adipose tissue; Lipids; Fourier transform infrared spectroscopy; Smoke avourings; Frequency; Absorbance; Oxidative degree;
Oxidation stability

1. Introduction
Pork adipose tissue is a traditional ingredient in the
processing of dry-fermented sausages such as Spanish
chorizo, in which it has an important role in the developing of the avour, texture and colour of the nal
product.
A major cause of deterioration of meat products is
lipid oxidation, either of lipids from meat muscle or
lipids from the animal fat added to the product as part
of its manufacture, which aects fatty acids in general
and polyunsaturated fatty acids in particular (Allen &
Allen, 1981; Fennema, 1993; Gray, 1978). The consequences of lipid oxidation have quality and toxic
implications (Shahidi, 1994); the former both due to the
loss of essential nutrients such as some fatty acids and
fat-soluble vitamins as well as to the generation of some
products which bring about undesirable changes in the
avour, colour, texture and functional properties of the
* Corresponding author. Tel.: +34-945-013081; fax: 34-945013014.
E-mail address: knpgulod@vf.ehu.es (M.D. Guillen).
0309-1740/$ - see front matter # 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/S0309-1740(03)00185-2

product; and the latter related to the formation of certain toxic by-products (Addis, 1986; Pearson, Gray,
Wolzak, & Horenstein 1983).
These changes in quality reduce the shelf-life of the
product and prevent consumer acceptance of oxidised
food (Gray & Pearson, 1994), therefore the prevention
of lipid oxidation in meat and meat products is of great
interest for the food industry. Many studies have indicated that lipid oxidation in meat products can be
eectively controlled or at least minimised by the use of
commercial synthetic antioxidants (Bailey, 1988; Gray
& Pearson, 1987). However, in view of the negative
public reaction to synthetic chemicals in foods, recent
studies have been focussed on the mechanism of stabilisation of meat lipids through vitamin E supplementation of animal diets (Onibi, Scaife, Murray, & Fowler,
2000a,2000b; Pfalzgraf, Frigg, & Steinhart, 1995; Phillips, Faustman, Lynch, Govoni, Hoagland, & Zinn,
2001; Wen, Morrissey, Buckley, & Sheehy, 1997). In
addition, some components used in the processing of
meat products have shown antioxidant properties; some
vegetal extracts (McCarthy, Kerry, Kerry, Lynch, &
Buckley, 2001; Tang, Kerry, Sheehan, Buckley, & Mor-

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M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

rissey, 2001; Tang, Sheehan, Buckley, Morrissey, &

Kerry 2001); nitrite used in curing meats (Han &
Yamauchi, 2000; Han, Yamauchi, & Park, 2000); and
smoke avourings used in smoking process of meat
products (Chomiak & Goryn, 1977; Coronado, Trout,
Dunshea, & Shah, 2002; Olsen, 1977; Schwanke, Ikins,
Kastner, & Brewer, 1996).
In order to assess the quality of the product as well as
to study the eect of antioxidants and food processing
on lipids, the measurement of lipid oxidation degree and
the determination of oxidative stability of meat or meat
products is a very important task. The usual methodology for studying the oxidative stability of lipids includes
a method for provoking the oxidation of the sample
under specic conditions, and the use of one or more
methods to determine parameters which give information about the oxidation degree reached. Numerous
analytical procedures for assessing lipid oxidation in
muscle foods have been described (Shahidi, 1994):
changes in fatty acids, the presence and type of free
radical intermediates, conjugated dienes and trienes,
polar components, trans-isomers, determination of
oxygen uptake, total or individual carbonyl compounds,
peroxide value (PV), 2-thiobarbituric acid (TBA) value,
anisidine value, uorescence and polarographic tests
and chromatographic determinations have all been
employed. However, the most common methods used in
meat and meat products lipid studies are chemical
measurement such as PV and TBA, the latter being the
most widespread procedure (Fernandez, Perez-Alvarez,
& Fernandez-Lopez, 1997; Shahidi, 1994). Both methods are not without drawbacks because they are not
always useful for determining oxidation degree for several reasons. Firstly, PV data are a measure of the
hydroperoxide concentration in the sample and their
determination takes a long time, involving great variations in many cases. This method is limited by the transitory nature of the hydroperoxides, which are
intermediate products in the formation of secondary
oxidation compounds (Fernandez et al., 1997; Gray,
1978). Secondly, TBA value is a measure of malonaldehyde concentration in the sample and has the
disadvantage that other compounds not formed as a
result of the oxidation process, or interfering compounds, can react with TBA. Another potential drawback to the TBA method is that malonaldehyde is often
bound to proteins and the conditions for its optimal
release are often hard to determine (Fernandez et al.,
1997; Shahidi, 1994). Therefore, the development of
new methods to determine oxidative stability as well as
oxidation degree of meat and meat products lipids are
needed.
Fourier transform infrared spectroscopy (FTIR) has
proved to be very helpful in the study and characterisation of edible fat and oils (Guillen & Cabo, 1997a,
1997b, 1998, 1999a), as well as in the study of their

degradation under oxidative conditions (Guillen &

Cabo, 1999b, 2000a, 2000b). In addition, changes
observed in the infrared spectra of edible oils have been
shown to be simultaneous with changes observed in
classic parameters such as peroxide value and anisidine
value (Guillen & Cabo, 2002). In this paper, the characterisation of the lipids of pork adipose tissue and the
monitoring of its degradation process, under oxidative
conditions, are carried out by means of Fourier transform infrared spectroscopy. In addition the eect of
smoking with two dierent liquid smoke avourings on
the oxidative stability of pork lipids is studied.

2. Material and methods

2.1. Samples, salting and smoking conditions
Pork adipose tissue of the same animal was acquired
in a local butchers shop. It was cut in right-angled
strips which were salted by covering them completely
with culinary salt for 24 h. After the salt was removed,
the strips were smoked by immersion in two liquid
smoke avourings, named LSA and LSB for 1 (LSA1 or
LSB1), 2 (LSA2 and LSB2), or 3 (LSA3 and LSB3) min
respectively. Composition of LSA and LSB had been
studied previously (Guillen & Ibargoitia, 1998; Guillen
& Manzanos, 1997). Unsmoked pork adipose tissue
strips submitted to the same sample preparation process
were used as control. The whole experimental procedure
was duplicated.
2.2. Sample oxidation
The unsmoked and smoked pork adipose tissue strips
were cut into small pieces and 10 g of each sample was
weighed into polystyrene Petri dishes. These were placed
in a Selecta convection oven at 70
C, with a stability of
 0.5%, without their lids in order to facilitate the
exposure of the sample to the circulating air. The oxidation of each samples was carried out in duplicate.
2.3. Spectral acquisition
The Fourier transform infrared spectra (FTIR) of the
melted lipids were acquired on a Bruker Vector 33
spectrometer interfaced to a personal computer operating under Windows NT. A lm of a small amount of
each sample (approximately 2 ml) was deposited
between two disks of KBr, avoiding the presence of air,
as in previous studies (Guillen & Cabo, 1997a, 1998,
1999a, 1999b, 2000a, 2000b, 2002). Duplicate spectra
were collected from each sample daily until it was
observed that the sample was in an advanced oxidation
stage. All spectra were recorded from 4000 to 500 cm1
with a resolution of 4 cm1. For each spectrum 32

M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

interferograms were co-added before Fourier transformation and zero-lled to give a data point spacing of
approximately 1.9 cm1. The measurement accuracy in
the frequency data is better than 0.01 cm1 due to the
laser HeNe internal reference of the instrument.
2.4. Study of the spectra
The frequency value for each band was obtained
automatically by the software. The height and area of
each band were measured in absorbance automatically
by means of a macro program taking two baselines:
37502472 and 1900530 cm1. These procedures avoid
the experimental errors associated with the subjectivity
of external operators. The assignation of the bands to a
specic functional group vibration mode was made by
comparison with previous studies of edible fats and oils
(Guillen & Cabo, 1997b).

3. Results and discussion

The FTIR spectrum of the lipids of pork adipose tissue is similar to that of other animal or vegetable fats
and oils studied before (Guillen & Cabo, 1997a, 1998)
because all of them consist mainly of triglycerides.
However, it shows some dierences either in the exact
frequency and absorbance of the bands or in the presence or absence of some bands due to dierences in
length and unsaturation degree of the acyl groups of the
triglycerides. Fig. 1 shows as an example the FTIR
spectrum of the melted fat of unsmoked pork adipose
tissue (control) before submission to oxidative conditions (day 0). Some of the most signicant bands together with a tentative assignment (Guillen & Cabo,
1997b) are the following: the weak band, near to 3471
cm1 assigned to the overtone of the glyceride ester
carbonyl absorption; the band near 30063007 cm1
due to the cis double-bond stretching vibration; the
bands at approximately 2925 and 2854 cm1 due to the
asymmetric and symmetric stretching vibrations of the
methylene functional group respectively; the band at
1746 cm1 due to the stretching vibration of the ester
carbonyl group of the triglycerides; the weak band near
1655 cm1 associated with the stretching vibration of
the carboncarbon double bonds of cis-disubstituted
olens; the band near 1464 cm1 due to the bending
vibrations of the CH2 and CH3 aliphatic groups; the
band near 1418 cm1 tentatively assigned to rocking
vibrations of the CH bonds of cis-disubstituted olens;
the band near 1377 cm1 due to symmetric bending
vibrations of the CH3 groups; the bands near 1237 and
1163 cm1 both associated with the stretching vibration
of the CO ester groups and with the bending vibration
of the CH2 group (Guillen & Cabo, 1997b) and both
related to the proportion of saturated acyl groups in oil

649

samples (Guillen & Cabo, 1997a); the bands at

approximately 1117 and 1099 cm1 associated with the
stretching vibration of the CO ester groups, the rst
being related inversely to the proportion of saturated
acyl groups in oil samples (Guillen & Cabo, 1997a); the
two weak bands near 966.5 and 910913 cm1; the rst
associated with bending vibration out of plane of isolated trans olens and the second dicult to assign; and
nally the band near 723 cm1 due to the overlapping of
the methylene rocking vibration of straight chain parans of the acyl groups and to the out-of-plane vibration of cis-disubstituted olens.
FTIR spectrum of the melted fat of smoked pork
adipose tissue (LSA or LSB), before submission to oxidative conditions, is identical to the spectrum of the
control sample because the salting and smoking process
had not signicantly changed the composition of the
samples. In general, under oxidative conditions FTIR
spectrum of melted fat of control sample show a pattern
of changes similar to that previously observed in dierent edible oils submitted to similar conditions (Guillen
& Cabo, 1999b, 2000a, 2000b). Fig. 1 illustrates the
most important spectral changes under oxidative conditions produced in melted fat of control sample at 0, 1, 2
and 4 days. The changes observed in the FTIR spectrum
of smoked samples submitted to oxidative conditions
are similar to those observed in control sample. The
dierence between unsmoked and smoked samples during the oxidation process are basically due to the rate at
which changes are produced; the rate of changes in the
FTIR spectrum of smoked samples is lower than in
unsmoked. A summary of these spectral changes is
given in Table 1.
3.1. Changes in the region between 3600 and 3100 cm1
The FTIR spectrum of control sample suers dierent changes in this region from day 1 of the experiment
(see Table 1). The band near 3471 cm1, originally due
to the overtone of the glyceride ester carbonyl absorption, becomes wider and more intense and its maximum
absorbance is shifted to lower wavenumbers near 3464
3465 cm1. The shifting and the broadening of this band
from 3600 to 3100 cm1 are due to overlapping of the
original band and of new absorptions caused by new
compounds generated as oxidation advances. Fig. 2a
shows the changes produced in this region of the FTIR
spectrum of control sample at dierent days of the oxidation. It can be observed that during days 1 and 2 the
broadening is mainly due to absorptions between 3460
and 3400 cm1 while from day 3 onwards the broadening is basically due to absorptions near 3530 cm1.
Dierent authors have assigned bands at approximately
3434, 3440 or 3458 cm1 to hydroperoxide groups generated in the oxidation process of dierent edible oils
(Guillen & Cabo, 1999b, 2000a; Van de Voort, Ismail,

M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

650

Fig. 1. FTIR spectra of melted fat of unsmoked pork adipose tissue (control) after 0, 1, 2 and 4 days under oxidative conditions.

Table 1
Days at which signicant changes are observed in the FTIR spectra of the samples under oxidative conditions
Samples

Broadening
36003100 cm1 (day)

Disappearance band
3006 cm1 (day)

Disappearance band
1655 cm1 (day)

Appearance band
987 cm1 (day)

Disappearance band
987 cm1 (day)

Appearance band
1630 cm1 (day)

Control
LSA1
LSA2
LSA3
LSB1
LSB2
LSB3

1
3
3
3
2
2
3

12
15a
14a
13a
13a
12a
15a

4
10
7
8
7
6
8

1
4
3
4
3
3
3

4
9
6
7
5
5
6

4
10
7
8
7
6
7

Remaining as a shoulder.

Sedman, & Emo, 1994). Absorptions near 3530 cm1

have been related to alcohols and to other compounds
derived from hydroperoxides (Ne, Frankel, & Weisleder, 1982); absorptions of free COOH groups of
hydroperoxi-epidioxides of methyl linolenate have been
described near 3520 cm1 and those of bonded C
OOH groups of the same compounds between 3150 and
3660 cm1. Therefore the beginning of the broadening
from 3600 to 3100 cm1 could be an indicator of the
beginning of the oxidation process in the samples. In
contrast, in all the smoked pork adipose tissue samples
there is a period of time in which the region from 3600
and 3100 cm1, and the frequency value of the band,
remain unaltered for several days while the sample is
under oxidative conditions, after which the broadening
and the shifting of the frequency of the band begin. For

samples LSA1, LSA2, LSA3 and LSB3 the delay is of 2

days and in samples LSB1 and LSB2 of 1 day (see
Table 1). Fig. 2b shows the changes observed in this
FTIR region in LSA3 sample and Fig. 3a represents the
evolution of the frequency value of the band near 3471
cm1 versus time for control, LSA3 and LSB3 samples
respectively. The beginning of the shifting of the frequency of this band coincides approximately with the
beginning of its broadening and could be considered as
an indicator of the beginning of the oxidation process.
The usefulness of changes in frequency value of dierent
bands of the spectrum of edible oils in order to study
their oxidation process has been previously reported
(Guillen & Cabo, 1999b). As Fig. 2b and Fig. 3a show,
smoked pork adipose tissue samples seem to have a
higher oxidative stability than the control sample.

M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

651

Fig. 2. (a) Region between 3600 and 3360 cm1 of the FTIR spectra of melted fat of control and (b) LSA3 samples at dierent days under oxidative
conditions.

As we have commented, changes are also observed in

the absorbance value of the band near 3471 cm1, for
this reason absorbance ratio values in which its absorbance is involved change throughout the oxidation process. That is the case of the ratio between the
absorbance of the band at 2854 cm1, due to the symmetrical stretching vibration of CH2 groups, and the
absorbance of the band between 3600 and 3100 cm1
(A2854/A36003100). This ratio maintains a value of

approximately 90100 in non-oxidized samples and suffers a sharp decrease when oxidation begins. In the
control sample the change in the value of the ratio A2854/
A36003100 is observed from day 1, while in the smoked
samples the ratio maintains a fairly constant value over
1 (LSB1 and LSB2 samples) or 2 (LSA1-3 and LSB3
samples) days, after which the value begins to decrease
until the sample is in a very advanced oxidation stage.
Fig. 4a shows the evolution of the ratio A2854/A36003100

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M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

Fig. 3. Frequency values of band near (a) 3471, (b) 3006 and (c) 966 cm1 respectively versus time for control, LSA3 and LSB3 samples under
oxidative conditions.

Fig. 4. Evolution of the ratio values (a) A2854/A36003100 and (b) A2854/A966975 respectively versus time for control, LSA3 and LSB3 samples under
oxidative conditions.

value for control sample and smoked samples LSA3 and

LSB3 in the course of the oxidation process. In general,
values below 90 indicate that oxidation has begun. In
addition the lower the value of this ratio the more
advanced is the oxidation in the samples. In previous
papers, the changes observed in the ratio values of different bands have also proved to be useful indicators of
the oxidation degree of some edible oil samples (Guillen
& Cabo, 2000a).
In short, the beginning of the broadening of the band,
which is reected in the beginning of the change in ratio
value A2854/A36003100, coincides to a great extent in time
with the beginning of the shifting of the frequency value
from 3471 cm1 to lower wavenumbers around 3464
cm1. The rate of the whole changes above mentioned

varies as a function of the rate of the oxidation of the

samples. In the control sample the oxidation process
begins 1 or 2 days before it occurs in the smoked samples. Therefore the smoking process seems to have contributed to increasing the oxidative stability of the
samples. Both the shifting of the frequency value of
band near 3471 cm1 and the changes in the value of the
ratio A2854/A36003100 could be considered as indicators
of the oxidative degree of the samples.
3.2. Changes in band at approximately 30063007 cm1
In the control sample submitted to oxidative conditions the band near 30063007 cm1, associated to the
stretching vibration of cis CHolenic groups, suers

M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

a decrease in its absorbance value and a shifting of the

frequency towards lower wavenumbers from day 1 of
the experiment (see Fig. 1). This fact is due to the
decrease of cis double bonds in the samples as a consequence of the start of the oxidation. However, in the
smoked samples the changes are between 1 (samples
LSB1 and LSB2) and 2 (samples LSA1-3 and LSB3)
days later. This behaviour can be seen in Fig. 3b which
shows the frequency value of band near 30063007
cm1 for the control sample and smoked samples LSA3
and LSB3 in the course of oxidation. Therefore, the
beginning of the shifting of the frequency value of this
band is an indicator of the decrease of cis double bonds
in the samples and can be considered as a measure of
their oxidative stability. Under the same oxidative conditions, the smoked samples seem to have a higher oxidative stability than the control sample. The decrease in
the absorbance continues progressively until the total
disappearance of the band (day 12 for control sample)
or just becomes a shoulder (days 1215) in the smoked
samples (see Table 1). This shows that the sample is at a
very advanced stage of the oxidation process.
As the absorbance decreases the ratio between the
absorbance of the band at 2854 cm1, due to symmetrical stretching vibration of CH2 groups, and the
absorbance of the band near 30063007 cm1 (ratio
A2854/A3006) also changes in the course of the oxidation.
The value of the ratio A2854/A3006 increases as a consequence of the decrease of the absorbance of band near
30063007 cm1. In the control sample a sharp increase
in the value of the ratio A2854/A3006 is observed from
day 1 of the experiment while in samples LSA3 and
LSB3 a slight increase is observed over days 1 and 2 and
then the increase is more intense. This fact indicates that
the rst change in the FTIR spectrum of the samples is
the decrease of the absorbance of band near 30063007
cm1 as a consequence of the decrease of cis double
bonds in the sample. The changes observed in the frequency value of this band as well as in the value of the
ratio A2854/A3006 again show that the oxidation rate is
higher in the control than in smoked samples. Both
could be considered as useful parameters for studying
the oxidative stability of the samples.
3.3. Signicant changes in the region between 1800 and
1000 cm1
The frequency and the absorbance of the band at
approximately 1746 cm1, due to the ester carbonyl
functional group of the triglycerides, also change during
the oxidation process. The frequency value suers a
shift towards lower wavenumbers around 1745 cm1; in
the control sample the shift is produced from day 1
while in smoked samples the frequency maintains a
generally constant value for 2 or 6 days and then begins
to decrease. This behaviour has been associated with the

653

appearance of saturated aldehyde functional groups

(Frankel, 1980; Hamilton, 1989), causing an absorption
at 1728 cm1 which overlaps with the band of the ester
functional group. There are also changes in the absorbance value of the band near 1746 cm1 but as in previous papers (Guillen & Cabo, 2000a) the changes in
absorbance ratio in which this band is involved are not
as good for monitoring the oxidation process as those
mentioned.
In addition, the band at approximately 1655 cm1,
which is associated with the stretching vibration of
CC groups undergoes a decrease of its absorbance
as the oxidation process advances (see Fig. 1). In the
control sample it decreases sharply from day 1 of the
experiment and disappears completely at day 4 (see
Table 1). In contrast, in smoked samples LSA and LSB
the absorbance decrease is produced in a progressive
way and the total disappearance of the band is between
2 or 6 days behind the control sample (see Table 1).
At very advanced stages of the oxidation a very weak
band appears at approximately 1630 cm1, which has
been assigned to a,b-unsaturated aldehydes and ketones
(Van de Voort et al., 1994) (see Fig. 1). The appearance
of this band coincides with the disappearance of the
band near 1655 cm1 (see Table 1). The evolution of
this spectral region has been represented in Fig. 5 for
the control sample (Fig. 5a) and smoked sample LSA3
(Fig. 5b) respectively. For the control sample the band
appears at day 4 of the experiment while in smoked
samples it appears between 2 or 6 days later. Therefore,
the smoking procedure seem to have delayed the generation of secondary oxidation products such as a,bunsaturated aldehydes and ketones.
The frequency and the absorbance of bands at
approximately 1163 and 1237 cm1, both associated
with the stretching vibration of the CO ester groups
and with the bending vibration of CH2 groups, and the
bands at 1117 and 1099 cm1, both associated with the
stretching vibration of the CO ester groups, also show
changes during the oxidation process of the samples.
The frequency value of band at 1237, 1163 and 1099
cm1 shifts to higher wavenumbers while the frequency
value of band at 1117 cm1 shifts to lower wavenumbers. These changes begin on day 1 of the experiment in the control sample and continue in a
progressive way until the end of the process. In contrast
in smoked samples the frequency maintains a constant
value for 1 or 2 days and then begins to change. In a
similar way, the absorbance of these bands undergoes
changes which are reected in the absorbance ratios in
which they take part. This is the case of the ratio between
the absorbance of the band at 2854 cm1 and the absorbance of the band at 1237, 1163, 1117 or 1099 cm1
(ratios A2854/A1237, A2854/A1163, A2854/A1117 or A2854/
A1099), respectively. In general, all these ratios suer a
similar pattern of changes; in the control sample the

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M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

Fig. 5. (a) Region between 1690 and 1600 cm1 of the FTIR spectra of melted fat of control and (b) LSA3 samples at dierent days under oxidative
conditions.

ratio value changes from day 1 while in smoked samples

the changes take place between 1 and 3 days later. Again,
the changes observed in both the frequency value of the
bands and the ratio values before mentioned could be
useful indicators of the oxidation degree of the samples.
3.4. Signicant changes in the region between 1000 and
600 cm1
In all samples, there appears a low intensity band near
987 cm1 which is associated with the bending vibration
of conjugated CH trans,trans- and/or cis,trans-olenic

groups (Chan & Levett, 1977a, 1977b; Privett, Lundberg, Khan, Tolberg, & Wheeler, 1953). It appears at
approximately the same time as the beginning of the
broadening between 3600 and 3100 cm1. Specically,
this band appears on day 1 in the FTIR spectrum of the
control sample and on days 3 or 4 in the dierent
smoked samples LSA or LSB. However, the disappearance of the band occurs on day 4 in the control
sample and between days 5 and 9 in smoked samples
LSA and LSB (see Table 1). This behaviour can be seen
in Fig. 6 which shows the evolution of the spectral
region between 1100 and 890 cm1 for control (Fig. 6a)

M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

655

Fig. 6. (a) Region between 1100 and 890 cm1 of the FTIR spectra of melted fat of control and (b) LSA3 samples at dierent days under oxidative
conditions.

and LSA3 (Fig. 6b) samples respectively on dierent

days of their oxidation process. Therefore, compounds
with conjugated double bonds are intermediate compounds in the oxidation process. This fact has been also
shown in the oxidation of dierent edible oils (Guillen
& Cabo, 1999b, 2000a).

The frequency and the absorbance of the band originally at 966.5 cm1, associated with bending vibrations of CH functional groups of isolated trans-olens,
increases at dierent rates, depending on the sample, as
the oxidation advances. In the control sample the frequency value of the band shifts to higher wavenumbers

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M.D. Guillen, N. Cabo / Meat Science 66 (2004) 647657

from day 1, reaching a value near 975 cm1 on the last

day of the experiment. Bands at wavenumbers near 976
cm1 have been assigned to secondary oxidation products such as aldehydes or ketones supporting isolated
trans-double bonds (Van de Voort et al., 1994). In contrast, in smoked samples the frequency of this band
maintains a fairly constant value for 1 (samples LSB1-2)
or 2 (samples LSA1-3 and LSB3) days after which the
shifting begins. Samples with frequency values for this
band higher than 966.5 cm1 have begun the oxidation
process, which is more advanced the higher the frequency. Therefore the frequency value of band originally near 966.5 cm1 could also be considered as an
indicator of oxidative stability. Fig. 3c shows the evolution of the frequency value of this band throughout the
oxidation of the control sample and smoked samples
LSA3 and LSB3, respectively. In addition, the absorbance of the band near 966.5 cm1 also increases during
oxidation. This change is reected in the value of the
ratio between the absorbance of band at 2854 cm1 and
the band between 966 and 975 cm1 (ratio A2854/
A966975). In the control sample it decreases since day 1
while in smoked samples it maintains a constant value
for 12 days and then begins to decrease. This behaviour can be seen in Fig. 4b showing the evolution of
this absorbance ratio for the control sample and LSA3
and LSB3 samples respectively during the oxidation
process. The ratio A2854/A966975 could also be considered as an indicative parameter of oxidation.

4. Conclusions
FTIR spectroscopy is a useful technique for monitoring the oxidation process of smoked or unsmoked pork
adipose tissue. The timing, either of the appearance or
disappearance of certain infrared bands, or of the shifting of the frequency value of some bands as well as of
the changes observed in certain absorbance ratios
between dierent bands, could be considered as an
indicator of the oxidative stability of the samples. All
the changes observed in the FTIR spectrum of pork
adipose tissue samples reect its oxidation stage. Liquid
smokes LSA and LSB have shown antioxidant activity
on the lipids of pork adipose tissue. Smoking with LSA
and LSB has increased the oxidative stability of the
samples in comparison to the control sample.

Acknowledgements
The authors gratefully acknowledge the nancial
support of the Ministerio de Ciencia y Tecnologa
MCYT (AGL2000-1696) and of the Universidad del
Pas Vasco (UPV 101.123-EB087/99 and 9/UPV
00101.125.13667/2001).

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