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Supercritical CO2 (SF-CO2) extracts of ground black pepper have been found superior in reducing
lipid oxidation of cooked ground pork compared to conventional extracts as measured by TBARS
and hexanal concentrations. Oleoresin extracted by SF-CO2 at 28 MPa (60 C) was most effective
in reducing hexanal concentration for up to 2 days. Essential oil extracted by SF-CO2 at 10 MPa
(60 C) and essential oil prepared by a conventional method were less effective as antioxidants
than ground black pepper, oleoresin extracted by SF-CO2, and oleoresin prepared by a conventional
method. TBARS and hexanal analyses were considered reliable indicators of meat flavor deterioration.
Keywords: Black pepper; essential oil; oleoresin; supercritical CO2 extraction; antioxidant
INTRODUCTION
Tipsrisukond et al.
Table 1. Characteristics of Pepper Volatile Oil Obtained
by Steam Distillation and SF-CO2a
SF-CO2
yield of oil
total terpene
hydrocarbons
monoterpenes
sesquiterpenes
oxygenated
hydrocarbons
steam
distillation
8 MPa
40 C
8 MPa
60 C
10 MPa
40 C
10 MPa
60 C
1.05
82.19
0.43
74.86
0.52
71.33
0.71
79.54
0.65
75.85
71.95
23.85
3.05
57.53
40.82
5.72
63.55
34.75
6.18
59.64
40.38
6.47
48.71
51.19
7.63
temperature were 230, 200, and 180 C, respectively. Desorption time was 5 min.
Analysis of Cooked Ground Pork Volatiles. The volatiles were analyzed by gas chromatography using a PerkinElmer model 8500 gas chromatograph (Perkin-Elmer Corp.,
Norwalk, CT) equipped with a flame ionization detector. The
chromatographic column used was a 50M SE-54 fused silica
capillary (Hewlett-Packard, Palo Alto, CA) with internal
diameter 0.32 mm and film thickness of 0.5 m. Helium
carrier gas flow rate was 3 mL/min with split ratio of 1:7.6.
Column oven temperature program of 35 C held for 5 min
and then 8 C/min to 220 C and 2.0 C/min to 250 C was
used. The data were analyzed using the built-in processor of
the gas chromatograph. Quantitation of volatiles was performed using relative peak areas compared to peak areas of
the internal standard. The isolated cooked ground pork
volatiles were tentatively identified using retention time as
compared to previous literature values (Bailey et al., 1987).
Determination of 2-Thiobarbituric Acid-Reactive Substances (TBARS). The TBARS test was carried out in
duplicate as per Tarladgis et al. (1960) and as modified by
Bailey et al. (1987). The TBARS values were expressed in mg
of malonaldehyde/kg of meat.
Statistical Analyses of Data. All statistical analyses of
the data were performed using the general linear model
procedure of Statistical Analysis System (SAS, 1989). All data
were analyzed in a completely randomized design using
analysis of variance for each experiment. The means comparison in each experiment was performed using least significant difference (LSD) at R ) 0.01. The correlation analysis
and linear regression between density and essential oil yield
and recovery of piperine were also performed at R ) 0.01 or
0.05, as well as between the content of hexanal and TBARS
values. The extractions and piperine determination experiment were conducted three times. The analyses of volatiles
and TBARS experiments were conducted twice. All results,
then, were pooled for statistical analysis. The analyses of EO
volatiles were conducted in duplicate after each extract was
mixed; therefore, the statistical analyses were not completed.
RESULTS AND DISCUSSION
9.85
5.52
2.85
4.67
3.68
3.29
20.33
13.33
9.73
13.64
12.58
11.35
35.47
36.64
31.43
32.74
32.50
31.01
17.70
18.22
20.13
16.03
16.81
26.01
3.15
2.74
2.04
2.89
2.68
1.63
45
oleoresin
piperine
oleoresin
piperine
oleoresin
piperine
oleoresin
piperine
4.60
35.7
4.93
36.7
5.44
37.6
5.43
39.4
temperature (C)
50
55
60
4.74
35.0
5.14
36.5
6.02
37.1
5.82
38.0
4.84
35.3
5.24
36.6
6.13
37.1
6.05
35.9
5.21
35.9
6.06
37.4
6.47
39.1
6.33
38.4
65
5.07
33.2
5.97
35.7
6.10
34.6
6.03
32.8
Tipsrisukond et al.
Figure 1. Changes in hexanal levels (a) and TBARS value (b) of cooked ground pork with black pepper oils and oleoresins from
SF-CO2 and conventional extractions during storage at 4 C for 8 days. Note: LSD ) 0.0663, 0.2447, 0.234, 0.4373, and 0.6067
for 0, 2, 4, 6, and 8 days, respectively, R ) 0.01 (a); LSD ) 0.05, 0.0112, 0.0095, 0.0141, and 0.0223 for 0, 2, 4, 6, and 8 days,
respectively, R ) 0.01 (b). Note: GB, EO1, EO2, EO3, OR1, OR2, OR3, and GP represent ground pork mixed with ground black
pepper, ground pork mixed with commercial essential oil, ground pork mixed with laboratory essential oil, ground pork mixed
with essential oil obtained from supercritical carbon dioxide extraction, ground pork mixed with commercial oleoresin, ground
pork mixed with laboratory oleoresin, and ground pork mixed with oleoresin obtained from supercritical carbon dioxide extraction,
and ground pork without extract or ground spice added, respectively.
In the present experiment, 4 hydrocarbons, 14 carbonyls, and 5 alcohols from all isolated volatiles were the
compounds that were reported to be related to lipid
oxidation products found in cooked pork (Ho et al.,
1994). The key volatiles detected by GC were pentanal,
hexanal, heptanal, octanal, and 2,3-octanedione. Hexanal was predominant among the aldehydes and gave the
most consistent results for interpretation of antioxidant
properties among treatments. Hexanal is the only
aldehyde that arises from both the 9- and 13-hydroperoxides of linoleate, which is the unsaturated fatty
acid found in the greatest concentration in pork (Shahidi
and Pegg, 1994). In addition, hexanal has been reported
to be one of the most potent flavor volatiles derived from
linoleic acid and has been related to warmed-over flavor
(Handley et al., 1997; Shahidi and Pegg, 1994; Shahidi,
1994). Despite its potential further degradation into
samples, possibly due to lesser monoterpene hydrocarbons (Figure 1a). Nonetheless, the increases in TBARS
during storage for up to 8 days were less after addition
of SF-CO2 EO as compared to conventional extracts
(Figure 1b). The large increase in hexanal concentration and TBARS of cooked ground pork mixed with
conventional EO extracts may be due to high thermal
oxidation products contained in extracts during production. Govindarajan (1977) reported that the ratio of
unsaturated fatty acids to saturated fatty acids in black
pepper was approximately 65:35%, and oleic and linoleic
acids were the most predominant. Therefore, the
elevated temperature during steam distillation in the
production of conventional black pepper EO can contribute to thermal oxidation of those unsaturated fatty
acids. The smallest increase in aldehyde level and
TBARS value after storage for 4 days was found in the
ground black pepper sample. These results agree with
those of Farrel (1990) and Govindarajan (1977) who
reported that spice extracts seem to possess less stability in providing flavor, color, and heat intensity than
ground spices. In addition, it may be because the spice
extracts used in the present experiment were not
encapsulated, resulting in less stability of the antioxidant compounds. A correlation between the content of
hexanal and TBARS value has been found (r ) 0.64, R
) 0.05). Shahidi et al. (1987) has also found that a
linear relationship existed between the TBA numbers
and hexanal levels of cooked ground pork.
CONCLUSIONS