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Meat Science
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / m e a t s c i
Rapid identication of pork for halal authentication using the electronic nose and gas
chromatography mass spectrometer with headspace analyzer
M. Nurjuliana a, Y.B. Che Man a,, D. Mat Hashim a, A.K.S. Mohamed b
a
b
Halal Products Research Institute, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor, Malaysia
Department of Food Science, Faculty of Food Science and Technology, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor, Malaysia
a r t i c l e
i n f o
Article history:
Received 15 July 2010
Received in revised form 31 January 2011
Accepted 22 February 2011
Keywords:
Authentication
Pork
Electronic nose
Surface acoustic wave
Principal component analysis
a b s t r a c t
The volatile compounds of pork, other meats and meat products were studied using an electronic nose and gas
chromatography mass spectrometer with headspace analyzer (GCMS-HS) for halal verication. The zNose
was successfully employed for identication and differentiation of pork and pork sausages from beef, mutton
and chicken meats and sausages which were achieved using a visual odor pattern called VaporPrint, derived
from the frequency of the surface acoustic wave (SAW) detector of the electronic nose. GCMS-HS was
employed to separate and analyze the headspace gasses from samples into peaks corresponding to individual
compounds for the purpose of identication. Principal component analysis (PCA) was applied for data
interpretation. Analysis by PCA was able to cluster and discriminate pork from other types of meats and
sausages. It was shown that PCA could provide a good separation of the samples with 67% of the total variance
accounted by PC1.
2011 Elsevier Ltd. All rights reserved.
1. Introduction
Testing of food products for the purpose of labeling and
authentication is necessary to avoid unfair competition and assure
consumer protection against fraudulent practices in the food industry.
One of the major issues concerning authenticity is where high value
raw materials are substituted with cheaper materials (Al-Jowder,
Kemsley, & Wilson, 1997) and especially in cases involving value
added products, where the potential nancial rewards for substitution
of cheaper ingredients are relatively high (Lai, Kemsley, & Wilson,
1995). Problems related to adulteration of meat species in ground and
comminuted products have been a widespread problem in some retail
markets, while meat species identication is a major global concern
(Murugaiah et al., 2009). Identication of the species of origin in meat
samples is relevant to consumers for several reasons. The fallout from
fraudulent substitution or adulteration will possibly lead to economic
losses, jeopardize the health of consumers who may have specic food
allergies and emotional disturbance due to religious reasons (Asensio,
Gonzlez, Garca, & Martn, 2008; Bonne & Verbeke, 2008; Ghovvati,
Nassiri, Mirhoseini, Moussavi, & Javadmanesh, 2009; Haunshi et al.,
2009).
The advance in food technology has resulted in the issues getting
more complicated where ingredients used in foods are more difcult
to understand by the consumers unless they are directly involved in
the related eld. Additionally, the task of food authentication cannot
639
Fig. 1. Typical electronic nose chromatogram of pork. SAW detector response for pork.
Table 1
Tentative identication of volatile compounds of raw pork from the electronic nose prole.
Peak
Kovat's indices
Compounds
Odor description
1
2
3
4
5
6
7
612
718
806
903
1000
1104
1207
Diacetyl
3-hydroxy-2-butanone
2-methyl-propanal
Heptanal
Trimethyl pyrazine
Nonanal
Decanal
Buttery
Buttery
Pungent
Fatty
Roasted
Soapy
Soapy
Table 2
Major volatile components of pork by HSGCMS.
Peak
Compounds
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
0.461
2.295
4.432
6.616
11.821
15.466
16.219
17.083
17.674
18.671
19.264
19.739
20.190
20.837
21.288
21.971
22.909
23.104
23.585
23.704
23.793
23.858
24.013
24.185
25.615
26.410
26.725
26.986
28.043
28.844
29.052
30.986
31.230
31.390
32.755
33.010
33.366
34.500
34.916
35.206
35.984
37.041
38.780
Phenol
Hexanal
2-Butanone
1-methoxyl-2-methyl-2-Pentanone
Heptanal
Benzaldehyde
Heptyl ester 1-heptanol
2-pentyl-furan
Octanal
1-Hexanol
2, 4-Dimethylamphetamine
2-Octenal
1-Octyl-triuroacetate
Butanal
Nonanal
Decyl ester
2-Heptadecenal
Pentasiloxane
Naphtalene
Acetic acid
3-methyl-3,5 tetrahydro-4-thiopyranone
Acetamide
Dodecane
Nitro-L-arginine
2-Decenal
2-Heptadecenal
2H-Pyran
2,4-Decadienal
2-Undecenal
Tetradecane
2, 4-Bis(hydroxylamino)-6-methylpyramidine
Pentadecane
1-Heptadecanamine
Sulfur
Thiophene-3-ol
Dodecane
Hexadecanal
Propenoic acid
Sulfurous acid
Hexadecanal
3, 5-di-tert-Butyl-4-hyroxybenzaldehyde
Octadecanal
2-Octamine
640
Fig. 2. Typical electronic nose chromatogram of pork sausage. SAW detector response for pork sausage.
such as high sensitivity, easy handling of signal, low power and long
term stability.
surface of the sensor, the frequency of the SAW will be altered and will in
turn affect the detection signal and allow the identication of the
contaminants. The ow rate of puried helium was xed at 3.0 mL/min.
The total cycle time per sample was 15 s.
Table 3
Tentative identication of volatile compounds of pork sausage from the electronic
nose prole.
Peak
Kovat's indices
Compounds
Odor description
1
2
3
4
5
6
7
8
9
10
11
12
13
435
646
657
709
754
820
925
1043
1140
1212
1255
1902
2100
Ethanal
2-methybutanal
2-methyl pentan-3-one
Ethyl propionate
2-pentanone
Butanoic acid
Hexanethiol
Phenylmethanol
-a-Prenchyl alcohol
5-methyl-2-furanaldehyde
(t)-(4s)-carvone
Isoeugenol
Octadecanoic acid
Pungent
Pungent
Mint
Ethereal
Rancid
Sulfur
Camphor
Almond
Caraway
Floral
Zhang et al., 2006). The two main aims of PCA are the reduction in the
number of variables and elimination of redundancy.
3. Results and discussion
The electronic nose was used for rapid qualitative detection and
discrimination of pork from other types of meat and meat products
while the gas chromatography mass spectrometer with headspace
analyzer (GCMS-HS) was used for aroma proling of pork and other
meats.
3.1. Volatile compounds of pork
The chromatographic proles of raw meat aroma of pork, beef,
mutton and chicken obtained by electronic nose are shown in Fig. 1.
The chromatogram from the electronic nose is a graphical display of
the derivative of the frequency change versus time. Each peak found
in this derivative plot corresponds to a specic volatile compound and
has a retention time (given in seconds) which is specic to the column
and analysis temperature. The area under the peak was correlated to
the compound concentration and was expressed in counts (cts). There
were 7 (peaks: 1, 2, 3, 4, 5, 6 and 7) common compounds for all meat
samples. However, each sample showed variations in the amount for
641
Fig. 3. VaporPrint of different meats and sausages. 2 dimensional olfactory images which provide the odor concentration and characteristic shape for each sample.
642
Fig. 3 (continued).
Fig. 4. Four different meats (score plot) in principal component analysis of the electronic nose data. Abbreviations: p1, p2, p3, Pork1, Pork2, Pork3; c1, c2, c3, Chicken1, Chicken2,
Chicken3; m1, m2, m3, Mutton1, Mutton2, Mutton3; b1, b2, b3, Beef1, Beef2, Beef3.
643
Fig. 5. Four different meats and 3 different sausages (score plot) in principal component analysis of the electronic nose data. Abbreviations: p1, p2, p3 Pork1, Pork2, Pork3; c1, c2, c3
Chicken1, Chicken2, Chicken3; m1, m2, m3 Mutton1, Mutton2, Mutton3; b1, b2, b3 Beef1, Beef2, Beef3; ps1, ps2, ps3, ps4, ps5 Pork sausage1, Pork sausage2, Pork sausage3, Pork
sausage4, Pork sausage5; cs1, cs2, cs3, cs4, cs5 Chicken sausage1, Chicken sausage2, Chicken sausage3, Chicken sausage4, Chicken sausage5; bs1, bs2, bs3, bs4, bs5 Beef sausage1,
Beef sausage2, Beef sausage3, Beef sausage4, Beef sausage5.
and hence both the identity (retention time) and the quantity (amount)
of the substance can be calculated using the software incorporated in the
device. Different meat and sausage samples showed variations in the
amounts of each compound and generate a unique and easily
recognizable image. The unique nature of this display is subjected to
the relative concentrations of several compounds making up the mix
while also quantifying the strength of each chemical compound within a
sample. However, to get an overall view of the complex data, principal
component analysis was carried out (Figs. 4 and 5).
3.2. Principal component analysis
Principal component analysis (PCA) as an unsupervised classication method to visualize the resemblance and difference among
different measurements in the data sets was used in order to structure
the data matrix. The meat samples were separated along the rst PC
Fig. 6. Seven electronic nose variables (loading plot) in principal component analysis of the electronic data.
644
which described 67% of the peak variations (Fig. 5) and showed seven
dened groups. Along the PC1 axis, pork, chicken, mutton, beef and
beef sausages were located with high positive scores but on the other
hand along the PC3 axis, chicken sausage had low positive scores
while pork sausage had low negative scores. This percentage appears
to sufciently dene a good model, especially for qualitative purposes.
Fig. 6 shows the loading plot with seven variables. Only four variables
(2, 4, 6 and 7) had a far Euclidean distance from the origin while the
remaining variables were considered as unimportant for discrimination (low loading values along PC1 and close to the origin). The high
positive correlation between peak 4 and PC1 indicated that the
volatile prole of pork contained a higher proportion of heptanal
(peak number 4) (Table 1). This indicates that the heptanal has a
major inuence upon the discrimination of pork from other types of
meats and sausages. This concurred with the observation of Shahidi
(1994) who reported that aldehydes are the major components
identied in the volatiles of cooked pork.
4. Conclusion
The ability of the zNose to qualitatively discriminate and cluster
among 4 common meat samples and 3 types of sausage was
demonstrated in this study. Measurements of the volatile compounds
by GCMS-HS were also employed which indicate that the electronic
nose has adequate selectivity and sensitivity to perform avor
detection in meats. With a total analysis of less than a minute and
requiring less than 5 g of sample, the electronic nose offers a rapid,
accurate, low cost and environmentally friendly tool for detection of
porcine based ingredients in foods and this is especially useful for
halal authentication and verication.
Acknowledgment
This research work was supported by Universiti Putra Malaysia
(Grant No. Research University Grant Scheme: 91033) awarded to
Professor Dr. Yaakob Bin Che Man. The authors are also greatly
indebted to Mr. Tibby Lim for his technical support, Dr. Marina Abdul
Manaf, Miss Syahariza Zainul Abidin and Mdm. Siti Munira Abduk
Razak for their assistance.
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