ARTICLE IN PRESS

International Dairy Journal 16 (2006) 750–761

www.elsevier.com/locate/idairyj

Changes in flavour volatiles of whole pasteurized milk as affected by

packaging material and storage time
Andreas E. Karatapanis, Anastasia V. Badeka, Kyriakos A. Riganakos,
Ioannis N. Savvaidis, Michael G. Kontominas
Laboratory of Food Chemistry and Technology, Department of Chemistry, University of Ioannina, Ioannina 45110, Greece
Received 10 November 2004; accepted 23 June 2005

Abstract

Changes in volatile profiles of whole pasteurized milk stored under fluorescent light at 4 1C, packaged in different containers were
monitored for a period of 7 days in a study designed to differentiate between light-induced oxidative and purely autoxidative effects
related to packaging material. Changes in volatiles were measured using solid-phase microextraction–gas chromatography/mass
spectroscopy, while microbiological and sensory analyses were used to assess milk quality. Two distinct patterns of milk flavour
deterioration were observed. In light-exposed samples, a light-induced oxidation mechanism prevailed while in light-protected
samples, an autoxidation mechanism was apparent. Under both conditions, the concentration of selected odorous compounds
increased with storage time. Microbiological data correlated poorly with both sensory and GC/MS data. Sensory data correlated
well with selected volatile compounds pointing to dimethyl disulphide, pentanal, hexanal and heptanal as potential markers of fresh
milk quality. Based on sensory analysis, the optimal shelf life of the whole pasteurized milk used in this study was approximately 5
days.
r 2005 Elsevier Ltd. All rights reserved.

Keywords: Milk flavour; Packaging material; Storage time

1. Introduction described as rancid, butyric, bitter flavour, (d) ‘‘micro-

Determination of milk off-flavours has been the
subject of numerous investigations (Badings & Neeter,
1980; Contarini & Povolo, 2002; Kim & Morr, 1996;
Marsili, 2003; Toso, Procida, & Stefanon, 2002; Urbach,
1990). According to the committee on off-flavour
nomenclature and reference standards of the American
Dairy Science Association (Shipe et al., 1978) off-
flavours in milk may be categorized as follows: (a)
‘‘heated flavour’’, described as cooked, caramelized and
scorched flavour, (b) ‘‘light-induced flavour’’, described
as burnt sunlight flavour, (c) ‘‘lipolyzed flavour’’,
Corresponding author. Tel.: +302651098342;
fax: +302651098795.
E-mail address: mkontomi@cc.uoi.gr (M.G. Kontominas).
bial flavour’’, described as acidic, bitter, fruity, malty,
putrid unclean flavour, (e) ‘‘oxidized flavour’’, described
as papery, cardboardy, metallic, oily, fish flavour, (f)
‘‘transmitted flavour’’, described as weedy, cowy, barny
flavour and (g) ‘‘miscellaneous flavour’’, described as
flat, chemical, foreign, lack of freshness, salty flavour.
Modern techniques employed to isolate and concen-
trate odour active compounds from the volatile fraction
of milk products prior to gas chromatography/mass
spectroscopy (GC/MS) analysis include: vacuum dis-
tillation, simultaneous steam distillation and extraction,
static headspace (HS), dynamic HS/purge and trap,
direct thermal desorption (Contarini & Povolo, 2002)
for solid and semi-solid samples and solid-phase
microextraction (Jung, Yoon, Lee, & Min, 1998;
Marsili, 1999a; Toso et al., 2002). In addition to the

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doi:10.1016/j.idairyj.2005.06.008
 ARTICLE IN PRESS
A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761
above techniques for the analysis of semi- and non-
volatile flavour compounds, considerable work has been
done with HPLC, supercritical fluid extraction and
supercritical fluid chromatography (Marsili, 2003).
Packaging can directly prevent the development of
light-induced off-flavour by protecting the product from
both light and oxygen (Schröder, 1982; Skibsted, 2000;
Vassila, Badeka, Kondyli, Savvaidis, & Kontominas,
2002). Apart from traditional glass bottles and coated
paperboard cartons, all-plastic containers have been
used for pasteurized milk packaging (Defosse, 2000;
Schröder, Scott, Bland, & Bishop, 1985). Problems with
all-plastic containers used in the studies cited above
included light transmission and oxygen permeability. It
should be noted, however, that oxidative reactions
(auto-oxidation) have been reported to take place in
milk packaged even in coated paperboard cartons which
were found to be more or less impermeable to oxygen
(Rysstad, Ebbesey, & Eggestad, 1998; Schröder et al.,
1985). More recently, polyethylene perephthalate (PET)
and coextruded high-density polyethylene (HDPE)
bottles have been used for fresh milk packaging (Bakish
& Hatfield, 1997; Cladman, Scheffer, Goodrich, &
Griffiths, 1998; van Aardt, Duncan, Marcy, Long, &
Hackney, 2001). PET has excellent mechanical proper-
ties, a good barrier to oxygen and reduces the adverse
effects of light on milk quality in the form of pigmented
bottles. On the other hand, pigmented HDPE bottles,
both monolayer and multilayer, at a higher thickness
than current PET, are finding their way into the fresh
milk packaging market. Both provide excellent conve-
nience through easy opening and reclosing, thus
minimizing recontamination (Cladman et al., 1998).
Many studies have reported off-flavour development
in milk at a given storage time, usually at the end of shelf
life of the product (Contarini & Povolo, 2002; Cormier,
Raymond, Champagne, & Morin, 1991; Jenq, Bassette,
& Crang, 1988; Leong, Harte, Partridge, Ott, &
Downes, 1992; Marsili, 1999b; Urbach & Milne, 1987;
Vallejo–Cordoba & Nakai, 1994). Limited information
exists in the literature on changes in flavour compounds
of milk as affected by storage time and packaging
conditions. Thus the objectives of the present study were
(1) to monitor HS volatiles of whole pasteurized milk
stored under refrigeration and fluorescent light as a
function of storage time and type of packaging material
and (2) to possibly relate changes in volatile compounds
to sensory and microbiological attributes of milk.
2. Materials and methods
2.1. Packaging materials
Six different packaging materials were evaluated with
respect to their potential effect on milk quality during
751
refrigerated storage. The six packaging materials in-
cluded: (1) a 0.5 L clear glass bottle, 800 mm in thickness,
(2) a 0.5 L clear PET bottle, 300–350 mm in thickness; (3)
a 0.5 L pigmented [PET+2% TiO2] bottle, 300–350 mm
in thickness; (4) a 0.5 L pigmented [HDPE+2% TiO2/
HDPE+4% carbon black pigment/HDPE+2% TiO2]
3-layer coextruded bottle, 550–600 mm in thickness; (5) a
0.5 L pigmented [HDPE +2% TiO2] monolayer
bottle and (6) a 0.5 L coated paperboard carton
consisting of polyethylene/board/polyethylene (20/395/
35 mm). Freshly pasteurized milk stored in clear glass
bottles (day 0 of storage) served as the control sample.
The white (TiO2) pigmented bottles were chosen on the
basis of consumer preference (White, 1985) with regard
to colour and their potential protective effect against
harmful incident light. The carbon black pigment has
been suggested (Schröder, 1982) for maximum protec-
tion against UV–VIS radiation, with both pigments
being approved by the Food and Drug Administration,
USA. Bottle (4) containing inner and outer white
coloured layers was white in colour. Monolayer and 3-
layer HDPE and PET bottles were produced by Argo
Ltd. (Athens, Greece) on an extrusion molding line
(Soplar SA, Switzerland) and an injection stretch blow
molding line (Nissei ASB, USA) respectively. Paper-
board carton blanks were supplied by Dodoni Ltd.
(Ioannina, Greece) and were produced by Variopack
(Homburg/Saar, Denmark).
2.2. Sample preparation and handling
Homogenized whole fat milk (3.5% fat) was obtained
from the dairy plant Dodoni Ltd. (Ioannina, Greece)
immediately after pasteurization (75 1C, 15 s). The milk
was aseptically dispensed into sterilized bottles and
coated paperboard cartons in the plant laboratory.
Bottles were sealed using polypropylene screw caps
while coated paperboard cartons were sealed on the
production line sealer. HS for both cartons and bottles
was between 50 and 60 mL. The filled containers were
transported to the laboratory in polystyrene foam ice
boxes packed in ice within 30 min of the filling process.
Bottles were stored at 470.5 1C for a period up to 7
days under perpendicular fluorescent light provided by
one Philips 55 W ‘‘cool white’’ fluorescent tube in a
commercial display floor type cabinet 70
200
70 cm3
(w
h
d) in dimensions bearing a glass door. The
fluorescent lamp produced 825750 lux on the side
surface of the containers, measured with a General
Electric light meter (Fairfield, CT, USA). Milk samples
(100 mL) were sampled from sealed containers at 1, 3, 5
and 7 days after initial packaging for physicochemical,
microbiological and sensory testing. Testing at day 0
was carried out on milk samples immediately after
packaging. On each sampling day, samples of the six
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752 A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761
different treatments were assayed with 3 replicates for
each treatment (n ¼ 3).
2.3. SPME– GC/MS analysis
Milk samples (8 mL), along with 10 mL of an internal
standard solution (20 mg mL1 4-methyl-2-pentanone)
and a micro-stirring bar were placed in a 20 mL glass
serum vial (20
72 mm) which was sealed with an
aluminum crimp cap provided with a needle-pierceable
polytetrafluroethylene/silicone septum. Solid-phase mi-
croextraction (SPME) was performed with a 75-mm
Carboxen/Polydimethylsiloxane (PDMS) fibre mounted
to a SPME manual holder assembly (Supelco, Belle-
fonte, USA). The sample vial was placed in a 50 1C
water bath and stirred at high speed. After allowing
5 min for the sample to equilibrate at 50 1C, the needle of
the SPME device was inserted into the vial through the
vial septum, and the plunger of the SPME apparatus
was pushed down to expose the Carboxen/PDMS fibre
to the vial HS. After 15 min of exposure time with
constant stirring, the fibre was retracted into the needle
assembly and removed from the vial.
2.4. GC/MS analysis conditions
GC analysis of volatile compounds adsorbed onto the
SPME fibre was carried out on a 60-m
0.25-mm-
internal diameter DB-5 (5% phenyl–94% dimethyl
arylene siloxane) fused-silica capillary column with a
film thickness of 1 mm (J&W Scientific, Folsom, USA).
Flow rate of the helium carrier gas was 0.8 mL min1. A
Hewlett-Packard 6890 series gas chromatograph
equipped with a Hewlett-Packard 5973 mass selective
detector was used. During the injection phase, the
injector was operated in the split mode (2:1 split ratio) at
a temperature of 250 1C. For thermal desorption, the
SMPE fibre remained in the injector for 5 min. The
initial column temperature was 40 1C. The column was
maintained at 40 1C for 10 min, heated to 140 1C at a
rate of 5 1C min1, heated to 220 1C at a rate of
8 1C min1 and held at 220 1C for 5 min. MS conditions
were as follows: source 230 1C; acquisition performed in
electron impact (EI) mode (70 eV) by 2.92 scans s1 and
the mass range used was mass/charge (m/z): 33–300. The
temperature of the transfer line was held constant at
220 1C. Peak identification was performed by compar-
ison of retention times and mass spectra of eluting
compounds to those of the Wiley library (Wiley275, J.
Wiley & Sons Ltd., West Sussex, England).
2.5. Physical tests
2.5.1. Light transmission measurements
Spectral transmission characteristics over the wave-
length range of 350–780 nm for all packaging materials
were measured with a Shimadzu model 210 UV–VIS
recording spectrophotometer (Rysstad et al., 1998).
2.5.2. Determination of oxygen transmission rates
Oxygen transmission rates for all packages (bottles
and cartons) were measured using the Oxtran 2/20
oxygen permeability tester (Mocon Controls, USA)
at a relative humidity (RH) of 60%, temperature of
22 1C (ASTM D-3985) and were expressed as
mL m2 day1 atm1.
2.5.3. pO2 measurements
Dissolved O2 in the milk sample (pO2) was carried out
using a microprocessor oximeter (WTW, OXI 96,
Weilheim, Germany) via direct emersion of the oximeter
probe into the milk sample.
2.6. Microbiological tests
To monitor possible microbial post-pasteurization
contamination of milk in the various containers,
standard plate counts were determined according to
the International Dairy Federation (IDF) standard No.
100 B (IDF, 1991a). Psychrotrophic counts were
determined according to the IDF standard No. 101 A
(IDF, 1991b).
2.7. Sensory evaluation
A panel of 17 individuals consisting of faculty and
graduate students were trained, in two sessions, to
differentiate between various off-flavours in milk
samples by preparing and evaluating common off-
flavour reference standards (light oxidized, plastic-
acetaldehyde and lack of freshness) (van Aardt et al.,
2001). Sensory data were collected between days 0 and 7
of storage. Milk samples (30 mL, 1474 1C) were
presented to panelists in individual sensory booths as
sets of three or four with a resting interval of 1 or 2 min
between sample sets. Panelists rated each sample for
intensity and type of off-flavour on a scale between 0
and 5, where a score of 5 corresponded to very good
flavour milk and a score of 0 corresponded to milk unfit
for consumption due to very strong off-flavours (IDF,
1987).
2.8. Statistical analysis
Data were subjected to analysis of variance using the
Excel 97 software program (Microsoft, CA, USA).
Where statistical differences were noted, differences
among packages were determined, using the least
significant difference (LSD) test. Significance was
defined at Po0.05.
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3. Results and discussion compounds, namely dimethyl disulphide and heptanal

3.1. Volatile compound determination
Volatiles produced in milk as a function of storage
time and packaging material are shown in Tables 1–6.
Given that the detector response factor for each
compound was not determined, the amounts of volatiles
reported in Tables 1–6 are only semi-quantitative and
will be therefore used to show only increasing/decreas-
ing trends for each compound.
Freshly pasteurized milk (Table 1, day 0) in contact
with glass resulted in the measurement of 19 com-
pounds, including hydrocarbons (7), ketones (4), esters
(3) alcohols (2), aldehydes (2) and sulphur compounds
(1). A similar profile of volatiles has been reported for
low fat cows’ milk at day 0 of storage by Marsili and
Miller (2001).
As shown in Table 1, in addition to the compounds
identified in freshly pasteurized milk, a number of
were produced from day 1 of storage, while 2,3-
octanedione, 2-heptanone, octanal and nonanal were
formed toward the end of the product shelf life.
Carbonyl compounds are the secondary products of
lipid photoxidation while dimethyl disulphide is both a
product of light exposure and a microbial metabolite
(Jung et al., 1998). Of the above compounds, 2,2,4-
trimethyl pentane, dimethyl disulphide, pentanal, hex-
anal and heptanal increased proportionally with time of
storage.
A similar volatile profile was observed for milk stored
in clear and TiO2 pigmented PET bottles (Tables 2 and
3). This was expected as the mechanism of milk
deterioration in the above packaging materials is
photo-oxidation. Photo-oxidation occurs in milk in the
presence of a photosensitizer such as riboflavin which
excites oxygen to its singlet state, a requirement for
oxygen to react with the unsaturated lipid moiety to
produce a hydroperoxide (Skibsted, 2000). The TiO2

Table 1
Volatile compound profile (mg mL1) of whole pasteurized milk packaged in clear glass as a function of storage time at 4 1C

Volatile compound tra (min) Quality factorb Days of storage Trendc

0 1 3 5 7
d e
Ethanol 6.53 72 0.69 0.72 0.84 0.63 1.00
Acetone 7.52 86 117.27 130.44 129.64 112.32 136.01
Dimethyl sulphide 8.72 97 1.52 1.57 1.53 1.13 1.79
1-Propanol 10.43 80 0.61 0.73 0.68 0.40 0.76
3-Methyl pentane 11.91 91 0.44 0.44 0.56 0.61 0.93
2-Butanone 12.63 86 17.85 21.32 20.26 18.05 20.97
Ethyl acetate 13.80 86 0.73 0.73 0.64 0.60 0.82
Chloroform 14.13 96 1.09 1.06 1.36 1.63 0.88
Propanoic acid ethyl ester 14.87 86 7.76 4.46 5.01 4.73 3.94
3-Methyl-2-butanone 16.59 72 0.46 0.55 0.64 0.48 0.53
Benzene 16.97 91 2.16 2.89 3.87 3.73 3.94
2-Pentanone 18.19 70 1.78 2.38 2.00 1.81 2.15
2,2,4-Trimethyl pentane 18.41 83 4.31 6.49 15.36 36.03 41.37 mm
Pentanal 18.78 80 2.10 2.13 2.63 4.31 7.02 m
Butyric acid methyl ester 20.27 95 2.70 3.94 3.10 2.73 2.90
4-Methyl-2-pentanone (i.s.) 21.25 91 25 25 25 25 25 i.s.
Dimethyl disulphide 22.59 90 UD 0.30 0.43 0.58 0.89 m
Toluene 23.01 94 0.74 0.81 2.59 2.61 2.91
Hexanal 24.35 90 0.28 0.73 1.67 4.27 5.55 mm
1-Hexanol 27.46 72 UD UD UD UD 0.25
Ethyl benzene 27.67 94 0.26 0.54 0.47 0.41 0.86
1,4-Dimethyl benzene 28.00 97 0.51 0.92 0.72 0.68 1.00
2-Heptanone 28.52 87 UD UD UD UD 0.18
Heptanal 29.03 88 UD 0.14 0.21 0.44 0.80 m
2-Heptenal 31.31 75 UD UD UD UD 0.17
2,3-Octanedione 32.10 71 UD UD UD 0.18 0.49
Octanal 32.92 73 UD UD UD UD 0.16
Nonanal 36.01 72 UD UD UD 0.10 0.18

m ¼ slight increase, k ¼ slight decrease, mm ¼ large increase, kk ¼ large decrease, i.s. ¼ internal standard, UD ¼ under detection limit.
a
Retention time.
b
Quality factor ¼ % matching of the experimental mass spectra against those found in the Wiley database.
c
Trends are designated as follows:
d
Tentatively identified on the basis of the Wiley275 library (J. Wiley & Sons Ltd., West Sussex, England).
e
Values are the mean of three determinations (n ¼ 3).
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754 A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761

Table 2
Volatile compound (mg mL1) profile of whole pasteurized milk packaged in clear polyethylene terephthalate (PET) as a function of storage time at
4 1C

Volatile compound tra (min) Quality factorb Days of storage Trendc

1 3 5 7
d e
Ethanol 6.53 72 0.77 0.82 0.76 0.51
Acetone 7.52 86 114.16 133.66 123.71 121.98
Dimethyl sulphide 8.72 97 1.49 1.61 1.34 1.40
1-Propanol 10.43 80 0.44 0.72 0.35 0.46
3-Methyl pentane 11.91 91 0.56 0.53 0.64 0.84
2-Butanone 12.63 86 18.75 19.89 19.72 20.31
Ethyl acetate 13.80 86 0.74 0.67 0.65 0.93
Chloroform 14.13 96 1.04 1.46 3.31 1.42
Propanoic acid ethyl ester 14.87 86 4.14 4.81 3.59 4.29
3-Methyl-2-butanone 16.59 72 0.59 0.50 0.60 0.51
Benzene 16.97 91 3.79 3.82 3.85 3.98
2-Pentanone 18.19 70 2.02 1.99 1.77 2.07
2,2,4-Trimethyl pentane 18.41 83 7.77 17.88 31.41 40.16 m
Pentanal 18.78 80 2.17 2.74 6.43 8.41 m
Butyric acid methyl ester 20.27 95 3.53 2.25 2.44 2.38
4-Methyl-2-pentanone (i.s.) 21.25 91 25 25 25 25 i.s.
Dimethyl disulphide 22.59 90 0.33 0.54 0.77 1.25 m
Toluene 23.01 94 1.17 1.65 2.36 2.41
Hexanal 24.35 90 0.79 1.84 4.91 10.67 mm
1-Hexanol 27.46 72 UD UD UD 0.24
Ethyl benzene 27.67 94 0.40 0.54 0.31 0.35
1,4-Dimethyl benzene 28.00 97 0.73 1.06 0.22 0.33
2-Heptanone 28.52 87 UD UD 0.15 0.23
Heptanal 29.03 80 0.13 0.23 0.58 1.79 mm
2-Heptenal 31.31 75 UD UD UD 0.21
2,3-Octanedione 32.10 71 UD UD 0.39 1.01
Octanal 32.92 73 UD UD UD 0.19
Nonanal 36.01 72 UD UD 0.09 0.23

m ¼ slight increase, k ¼ slight decrease, mm ¼ large increase, kk ¼ large decrease, i.s. ¼ internal standard, UD ¼ under detection limit.
a
Retention time.
b
Quality factor ¼ % matching of the experimental mass spectra against those found in the Wiley database.
c
Trends are designated as follows:
d
Tentatively identified on the basis of the Wiley275 library (J. Wiley & Sons Ltd., West Sussex, England).
e
Values are the mean of three determinations (n ¼ 3).

pigmentation in the white coloured bottle only partly
protects the product from photo-oxidation resulting
in lower amounts of pentanal, dimethyl disulphide,
hexanal and heptanal, as well as 2-heptanone, octanal,
and nonanal after day 7 of storage. This is in agree-
ment with the findings of de Man (1978) who reported
that inorganic fillers (TiO2) used to block harmful
light wavelengths were not effective in preventing
light-induced deterioration of milk. This may be
due to the fact that filler particles may act as
strong scattering centers causing a large proportion of
incident light to find its way into the milk at scattered
angles.
The present results are in agreement with earlier
reports in the literature (Cadwallader & Howard, 1998;
Cladman et al., 1998) that showed the most common
volatile compounds in light-oxidized milk to be dimethyl
disulphide, pentanal, hexanal, acetaldehyde, 1-hexen-3-
one and 1-octen-3-one. The latter two compounds were
not detected in the present study. Furthermore, neither
acetaldehyde, a degradation product of PET, nor its
oxidation product, acetic acid, was identified in milk
packaged in the PET bottles. This is in contrast to the
findings of van Aardt et al. (2001), Nijssen, Kamper-
man, and Jetten (1996) and Bosset, Gallmann, and
Sieber (1994). The reason for this is unclear. Cadwalla-
der and Howard (1998) attributed off-flavours at the
end of milk shelf life to compounds such as 2,3-
butanedione. In the present study, a similar compound
in structure (2,3-octanedione) was identified on day 5 of
milk storage (Tables 1–3). Marsili (1999a) used SPME
for isolation of milk volatiles and reported a linear
relationship between hexanal formation in 2% cows’
milk packaged in half gallon HDPE jugs exposed to
fluorescent light for 2 days. A plot of increasing
pentanal concentration with increasing time of exposure
more accurately fitted a second-order polynomial
equation.
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Table 3
Volatile compound profile (mg mL1) of whole pasteurized milk packaged in monolayer pigmented polyethylene terephthalate (PET) as a function of
storage time at 4 1C

Volatile compound tra (min) Quality factorb PET days of storage Trendc

1 3 5 7
d e
Ethanol 6.53 72 0.91 0.76 0.88 0.85
Acetone 7.52 86 131.65 123.16 134.32 123.42
Dimethyl sulphide 8.72 97 1.66 1.40 1.49 1.44
1-Propanol 10.43 80 0.77 0.70 0.62 0.73
3-Methyl-pentane 11.91 91 0.38 0.60 0.51 0.33
2-Butanone 12.63 86 21.26 19.66 19.48 19.50
Ethyl acetate 13.80 86 0.82 0.72 0.65 0.69
Chloroform 14.13 96 1.10 1.48 1.87 1.61
Propanoic acid ethyl ester 14.87 86 4.25 4.33 3.88 3.34
3-Methyl-2-butanone 16.59 72 0.69 0.58 0.53 0.57
Benzene 16.97 91 3.49 3.88 3.28 2.81
2-Pentanone 18.19 72 2.49 1.92 1.85 1.86
2,2,4-Trimethyl-pentane 18.41 83 11.79 16.61 35.41 41.86 m
Pentanal 18.78 80 2.05 2.61 4.08 6.43 m
Butyric acid methyl ester 20.27 95 3.65 2.36 2.53 2.05
4-Methyl-2-pentanone (i.s.) 21.25 91 25 25 25 25 i.s.
Dimethyl disulphide 22.59 90 0.30 0.36 0.45 0.78 m
Toluene 23.01 94 1.02 1.84 2.06 1.89
Hexanal 24.35 90 0.71 1.54 3.96 5.14 mm
1-Hexanol 27.46 72 UD UD UD 0.26
Ethyl benzene 27.67 94 0.30 0.42 0.29 0.29
1,4-Dimethyl benzene 28.00 97 0.37 0.52 0.40 0.40
2-Heptanone 28.52 87 UD UD UD 0.17
Heptanal 29.03 80 UD 0.17 0.36 0.74 m
2-Heptenal 31.31 75 UD UD UD 0.15
2,3-Octanedione 32.10 71 UD UD 0.25 0.62
Octanal 32.92 73 UD UD UD 0.14
Nonanal 36.01 72 UD UD UD 0.15

m ¼ slight increase, k ¼ slight decrease, mm ¼ large increase, kk ¼ large decrease, i.s. ¼ internal standard, UD ¼ under detection limit.
a
Retention time.
b
Quality factor ¼ % matching of the experimental mass spectra against those found in the Wiley database.
c
Trends are designated as follows:
d
Tentatively identified on the basis of the Wiley275 library (J. Wiley & Sons Ltd., West Sussex, England).
e
Values are the mean of three determinations (n ¼ 3).

The present results differ significantly from those of
Urbach and Milne (1987) who found major differences
in the concentration of ethanol, acetaldehyde, propan-2-
ol and acetone between freshly pasteurized milk and
milk held for 7 days at 7 1C. In the present study,
acetone concentrations remained quite constant
throughout the 7-day storage period while the ethanol
concentration increased on day 7 of storage and in O2
permeable packages (Tables 4–6). Acetaldehyde and
propan-2-ol were not detected. Finally, Jenq et al. (1988)
reported that both n-hexanal and n-pentanal were the
compounds in milk most affected by fluorescent light
(51 h exposure) and added copper.
A different profile of volatiles produced during milk
storage was observed (formation of non-oxidation
products) in light protected containers; 33 compounds
in milk samples packaged in 3-layer pigmented HDPE
bottles, 32 compounds in milk samples packaged in
TiO2 pigmented HDPE bottles and 36 compounds in
milk samples packaged in carton packs were tentatively
identified (Tables 4–6). Milk samples (4–6) in light-
protected containers had significantly lower levels of
oxidation than those packaged in the light-exposed
containers (1–3).
An important observation was that dimethyl disul-
phide, a product mainly of milk light exposure was not
detected (Table 4), indicative of the protective effect of
the multilayered HDPE bottle provided by the carbon
black pigment. The same compound was formed in
small amounts in pigmented HDPE bottles (Table 5)
and even lower amounts in carton packs (Table 6). The
carton pack provided a somewhat better protection of
milk than the pigmented HDPE bottle from incident
light. This is supported by light transmittance data of
packaging materials (Fig. 1). Another important ob-
servation (Table 4) was that carbonyl compounds,
formed as secondary autoxidation products such
as pentanal, hexanal, 2-heptanone, 2-pentanone and
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756 A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761

Table 4
Volatile compound profile (mg mL1) of whole pasteurized milk packaged in 3-layer pigmented high-density polyethylene (HDPE) as a function of
storage time at 4 1C

Volatile compound tra (min) Quality factorb Days of storage Trendc

1 3 5 7

Ethanold
6.53 72 0.83 e
0.87 1.04 13.20 mm
Acetone 7.52 86 126.74 133.87 132.76 146.91
Dimethyl sulphide 8.72 97 1.66 1.60 2.19 19.33 mm
Methyl acetate 9.04 70 0.46 0.19 0.53 0.83 m
Dichloro-methane 9.25 97 UD UD 7.52 18.67
Carbon disulfide 9.66 83 UD 1.29 1.16 1.62
2-Methyl-propanol 10.48 70 0.75 1.03 1.75 1.81
3-Methyl-pentane 11.91 91 0.94 0.80 0.61 1.29
2-Butanone 12.63 87 20.44 26.63 21.39 21.31
Ethyl acetate 13.80 86 0.89 0.91 0.73 3.61 mm
Chloroform 14.13 96 0.89 1.35 3.70 4.42 m
Propanoic acid ethyl ester 14.87 86 4.64 9.05 15.21 12.68
3-Methyl-butanal 16.30 97 UD UD UD 1.68
3-Methyl-2-butanone 16.59 72 0.55 0.67 0.66 0.76
Benzene 16.97 91 4.54 4.71 4.03 4.88
2-Pentanone 18.19 72 2.16 2.55 1.93 2.49
2,2,4-Trimethyl-pentane 18.41 83 9.61 39.53 148.28 23.20 mmkk
Pentanal 18.78 80 1.85 2.28 2.33 2.91
Butyric acid methyl ester 20.27 97 2.96 3.01 2.47 6.17 m
3-Methyl-1-butanol 20.86 78 UD UD UD 1.24
4-Methyl-2-pentanone (i.s.) 21.25 91 25 25 25 25 i.s.
Dimethyl disulphide 22.59 90 UD UD UD UD
Toluene 23.01 94 1.25 1.92 2.47 4.24 m
Hexanal 24.32 90 0.48 0.54 0.80 UD
Butyric acid ethyl ester 24.35 97 UD UD UD 6.57
Ethyl benzene 27.67 94 0.53 0.45 0.38 0.72
1,4-Dimethyl benzene 28.00 97 1.20 0.86 0.66 1.31
2-Heptanone 28.52 87 — 0.12 0.10 0.24
1,3-Dimethyl benzene 29.12 97 0.63 0.31 0.39 0.43
Hexanoic acid methyl ester 29.87 90 0.22 UD UD 1.52
Hexanoic acid ethyl ester 32.61 97 UD UD UD 2.83
Limonene 34.19 98 UD 0.10 UD 0.20
Octanoic acid methyl ester 36.40 75 UD UD UD 0.19
Nonanal 36.01 72 0.09 0.11 0.11 0.19

m ¼ slight increase, k ¼ slight decrease, mm ¼ large increase, kk ¼ large decrease, i.s. ¼ internal standard, UD ¼ under detection limit.
a
Retention time.
b
Quality factor ¼ % matching of the experimental mass spectra against those found in the Wiley database.
c
Trends are designated as follows:
d
Tentatively identified on the basis of the Wiley275 library (J. Wiley & Sons Ltd., West Sussex, England).
e
Values are the mean of three determinations (n ¼ 3).

3-methyl-2-butanone, remained constant in concentra-
tion equivalent to concentrations in freshly pasteurized
milk (day 0 of storage). This was expected since photo-
oxidation did not progress to any significant extent
owing to the excellent protection provided by the carbon
black pigment. Christy, Amantea, and Irwin (1981)
demonstrated that co-extruded black/white polyethylene
totally blocked diffuse transmittance of 400–500 nm to
less than 5% thus protecting milk from off-flavour
development. The same observations hold more or less
for the other two samples packaged in TiO2 pigmented
HDPE and paperboard carton containers (Tables 5
and 6). A partial exception to this trend was the slight
increase in pentanal and hexanal concentrations with
increasing storage time observed for milk packaged in
the TiO2 pigmented HDPE bottle. This effect could be
explained in terms of the partial protection of milk from
light provided by this packaging material (Fig. 1).
Excess production of ethanol in milk packaged in PE
bottles and carton packs (Tables 4–6) was responsible
for the formation of large amounts of esters such as
butyric acid methyl ester, butyric acid ethyl ester,
hexanoic acid methyl ester, hexanoic acid ethyl ester
and octanoic acid methyl ester. Such esters were not
found in milk packaged in glass and PET bottles. This
route of ester formation has been suggested by Hosono,
Elliot, and McGugan (1974) and is related to growth of
Pseudomonas spp., P. fragi in particular. Toluene may
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Table 5
Volatile compound profile (mg mL1) of whole pasteurized milk packaged in monolayer pigmented high-density polyethylene (HDPE) as a function
of storage time at 4 1C

Volatile compound tra (min) Quality factorb Days of storage Trendc

1 3 5 7

Ethanold
6.53 72 0.75 e
0.69 0.46 10.62 mm
Acetone 7.52 86 126.12 127.75 114.58 154.55
Dimethyl sulphide 8.72 97 1.61 1.60 1.26 37.17 mm
Methyl acetate 9.04 70 0.45 0.58 0.37 1.53 m
Dichloro-methane 9.25 97 UD UD 2.08 1.85
Carbon disulfide 9.66 83 UD 0.53 0.27 0.62
2-Methyl-propanol 10.48 70 0.74 0.67 0.52 0.51
3-Methyl-pentane 11.91 91 0.62 0.60 0.39 0.49
2-Butanone 12.63 87 20.96 20.58 18.23 16.08
Ethyl acetate 13.80 86 0.89 0.67 0.58 5.61 mm
Chloroform 14.13 96 1.04 0.98 2.89 1.26
Propanoic acid ethyl ester 14.87 86 4.36 4.81 3.81 4.75
3-Methyl-butanal 16.30 97 UD UD UD 0.57
3-Methyl-2-butanone 16.59 72 0.63 0.63 0.57 0.63
Benzene 16.97 91 4.13 4.15 3.08 4.20
2-Pentanone 18.19 72 2.26 2.05 1.54 2.74
2,2,4-Trimethyl-pentane 18.41 83 11.17 19.73 146.92 2.36 mmkk
Pentanal 18.78 80 2.06 2.93 3.42 4.06 m
Butyric acid methyl ester 20.27 97 2.53 2.17 2.40 9.19 m
3-Methyl-1-butanol 20.86 78 UD UD UD 3.06
4-Methyl-2-pentanone (i.s.) 21.25 91 25 25 25 25 i.s.
Dimethyl disulphide 22.59 90 UD 0.34 0.42 0.60
Toluene 23.01 94 1.40 2.53 1.74 2.15
Hexanal 24.32 90 0.58 0.87 1.45 —
Butyric acid ethyl ester 24.35 97 UD UD UD 2.33
Ethyl benzene 27.67 94 0.46 0.34 0.56 0.84
1,4-Dimethyl benzene 28.00 97 0.43 0.60 1.59 1.86 m
2-Heptanone 28.52 87 UD UD UD 0.38
1,3-Dimethyl benzene 29.12 97 0.43 0.23 0.49 0.76
Hexanoic acid methyl ester 29.87 90 0.32 UD UD 3.21
Hexanoic acid ethyl ester 32.61 97 UD UD UD 1.26
Octanoic acid methyl ester 36.40 75 UD UD UD 0.43
Nonanal 36.01 72 0.09 0.12 0.13 0.28

m ¼ slight increase, k ¼ slight decrease, mm ¼ large increase, kk ¼ large decrease, i.s. ¼ internal standard, UD ¼ under detection limit.
a
Retention time.
b
Quality factor ¼ % matching of the experimental mass spectra against those found in the Wiley database.
c
Trends are designated as follows:
d
Tentatively identified on the basis of the Wiley275 library (J. Wiley & Sons Ltd., West Sussex, England).
e
Values are the mean of three determinations (n ¼ 3).

originate from the breakdown of b-carotene as well as
other sources (Marsili & Miller, 1998) while chloroform
may be from chlorinated sanitizers used to wash teats
prior to milking. The formation of 3-methyl butanal is
believed to be through the action of bacterial enzymes
on leucine (Marsili & Miller, 1998).
3.2. Microbiological analysis
statistically significant differences (P40:05) in mesophi-
lic counts were recorded for milk samples in all
packaging materials for a given sampling day during
the entire 7-day storage period (data not shown). After 7
days for storage, mesophilic counts were between 6.00
and 6.41 log cfu mL1, values close to the upper limit
(106–107 cfu mL1) for keeping quality of milk (IDF,
1986).

3.2.1. Mesophilic counts 3.2.2. Psychrotrophic counts

Initial (day 0) counts were high, 4.36 log cfu mL1,
indicative of the current poor milk collection practices
throughout Greece. Such high microbial loads are
responsible for the short shelf life of domestic refriger-
ated milk, which does not normally exceed 5 days. No
Initial (day 0) counts were 3.43 log cfu mL1. No
statistically significant (P40:05) differences in psychro-
trophic counts were recorded for milk samples in all
packaging materials up to day 3 of storage
(3.67 log cfu mL1). Statistically significant (Po0:05)
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758 A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761

Table 6
Volatile compound profile (mg mL1) of whole pasteurized milk packaged in paperboard carton as a function of storage time at 4 1C

Volatile compound tra (min) Qulaity factorb Days of storage Trendc

1 3 5 7

Ethanold 6.53 72 0.59e 0.79 0.45 3.98 mm

Acetone 7.52 86 128.61 132.97 134.51 121.34
Dimethyl sulphide 8.72 97 1.60 1.42 1.16 13.57 mm
Methyl acetate 9.04 70 0.53 0.49 0.42 1.69 m
Dichloro-methane 9.25 97 — — 18.27 21.14
Carbon disulfide 9.66 83 0.61 1.81 2.20 2.81
2-Methyl-propanol 10.48 70 0.73 0.81 0.65 1.16
3-Methyl-pentane 11.91 91 0.94 0.51 0.67 0.71
2-Butanone 12.63 87 20.90 20.27 20.00 15.68
Ethyl acetate 13.80 86 0.46 0.55 0.74 44.06 mm
Chloroform 14.13 96 2.50 3.23 7.56 6.38
Propanoic acid ethyl ester 14.87 86 6.46 10.51 11.24 14.81 m
3-Methyl-butanal 16.30 97 — — — 2.08
3-Methyl-2-butanone 16.59 72 0.57 0.56 0.46 0.84
Benzene 16.97 91 4.31 4.11 3.46 5.03
2-Pentanone 18.19 72 2.53 2.08 1.69 2.64
2,2,4-Trimethyl-pentane 18.41 83 5.55 17.14 37.75 17.57 mmkk
Pentanal 18.78 80 1.80 2.31 3.12 2.61
Propanoic acid methyl ester 19.76 72 — — 0.13 1.84
Butyric acid methyl ester 20.27 97 4.24 3.09 3.06 6.25
3-Methyl-1-butanol 20.86 78 — — — 2.96
4-Methyl-2-pentanone (i.s.) 21.25 91 25 25 25 25 i.s.
Dimethyl disulphide 22.59 90 — — 0.14 0.23
Toluene 23.01 94 1.66 2.59 5.34 4.57
Hexanal 24.32 90 0.60 0.61 1.12 —
Butyric acid ethyl ester 24.35 97 — — — 10.74
Ethyl benzene 27.67 94 2.08 1.08 1.21 1.87
1,4-Dimethyl benzene 28.00 97 7.00 4.15 4.01 6.04
2-Heptanone 28.52 87 — — — 0.54
1,3-Dimethyl benzene 29.12 97 3.28 3.38 1.97 2.55
Hexanoic acid methyl ester 29.87 90 0.41 0.19 0.14 1.44
a-Pinene 30.95 97 0.70 0.60 0.67 1.38
Hexanoic acid ethyl ester 32.61 97 — — 0.12 3.80
1,3,5-Trimethyl benzene 33.04 93 — — — 0.32
Delta.3carene 33.65 97 0.38 0.32 0.41 0.76
Limonene 34.19 98 — — 0.09 0.52
Octanoic acid methyl ester 36.40 75 — — — 0.22

m ¼ slight increase, k ¼ slight decrease, mm ¼ large increase, kk ¼ large decrease, i.s. ¼ internal standard.
a
Retention time.
b
Quality factor ¼ % matching of the experimental mass spectra against those found in the Wiley database.
c
Trends are designated as follows:
d
Tentatively identified on the basis of the Wiley275 library (J. Wiley & Sons Ltd., West Sussex, England).
e
Values are the mean of three determinations (n ¼ 3).

differences among packages were recorded during days 5
and 7 of storage (data not shown). After 7 days of
storage, relatively high psychrotrophic counts between
5.31 and 6.10 log cfu mL1 were recorded for all packa-
ging materials.
3.3. Sensory evaluation
Flavour evaluation results are shown in Table 7. In
general, off-flavours increased more rapidly in milk
packaged in light-exposed containers compared with
light-protected containers. After 5 days of storage, the
milk sample in the multilayer (white/black/white)
HDPE bottle received a score of 4.1 (best protection)
followed by the sample in the paperboard carton (score
3.6), the sample in the monolayer pigmented HDPE
bottle (score 3.4) and the sample in the clear glass bottle
(score 3.0), with the samples in clear and pigmented PET
scoring 2.5 and 2.7, respectively. Flavour defects were
described as ‘‘slightly stale’’ to ‘‘stale’’ and ‘‘fruity’’ for
samples packaged in paperboard carton and HDPE and
‘‘plastic’’, ‘‘oxidized’’ to ‘‘burnt taste’’ for samples
packaged in PET and glass bottles. After 7 days of
storage, the milk samples in all containers were
 ARTICLE IN PRESS
A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761 759

unacceptable. The present sensory results are in general
agreement with those of van Aardt et al. (2001) who
reported better milk keeping quality in amber PET and
UV compounded PET compared with clear PET bottles
as well as the results of Cladman et al. (1998) who
reported superior milk protection against light oxidation
when milk was packaged in green PET in comparison
with clear PET bottles. Even though the total microbial
count (106–107 cfu mL1) was in all cases below or equal
to the approximate upper limit for acceptability after 7
days of storage, the sensory characteristics of the
product had clearly deteriorated resulting in an unac-
ceptable product. This has previously been noted by
Labuza (1982) and Maxcy and Wallen (1983) who
reported that the most reliable method to judge the
quality of fresh milk is sensory evaluation.
100
90
80
70
60
%T
3.4. Relationship between sensory, microbiological and
volatile compound data
There was a rather poor relationship between sensory
and microbiological data with respect to both total
mesophile and psychrotroph counts. As previously
documented (Bishop & White, 1986; Marsili, 2000;
Urbach & Milne, 1987), spoilage of a specific food
substrate is the result of growth of specific spoilage
organisms and not of total microflora. Furthermore,
there was a poor relationship between microbiological
and volatile compound data since for a large number of
volatiles there was no change in concentration with
increasing microbial populations (i.e. between days 5
and 7 of storage, Tables 1–6).
With regard to the relationship between sensory and
volatile compound data several observations can be
made. In containers where light-induced changes pre-
dominate (containers 1, 2 and 3) there was a gradual
increase in the concentration of pentanal, hexanal,
1 heptanal, dimethyl disulphide and 2,2,4-trimethyl
2
Table 8
Oxygen transmission rate of packaging materials
Packaging materiala O2 transmission rateb

50
(mL m2 d1 atm1)
40
Clear glass bottle 0
30 Clear PET bottle 15.471.1a
3
20 Pigmented PET bottle 13.271.2a
3-Layer pigmented, coextruded 42.272.4b
10 5 HDPE bottle
6 Monolayer pigmented HDPE 44.472.5b
0 4
300 350 400 450 500 550 600 650 700 750 800 bottle
λ (nm) Coated paperboard carton 824742c

Fig. 1. Spectral transmission curves of the milk packaging materials. a

(1) Clear glass, (2) clear polyethylene terephthalate (PET), (3)
pigmented PET, (4) 3-layer pigmented high-density polyethylene
(HDPE), (5) monolayer pigmented HDPE and (6) coated paperboard
carton (T ¼ transmittance, l ¼ wavelength).
HDPE ¼ high-density polyethylene, PET ¼ polyethylene ter-
ephthalate, temperature ¼ 22 1C, relative humidity ¼ 60%.
b
Values within a column followed by different superscript letters are
significantly different (Po0:05). Values reported are the mean of six
replicates 7SD.

Table 7
Flavour evaluation of whole pasteurized milk packaged in various containers during storage at 4 1C

Packaging materiala Scoreb/comments

Days of storage at 4 1C

0 1 3 5 7

Clear glass bottle 5a,* 5a 3.5c/Slightly stale 3.0c/Slight oxidized flavour 1.8b/Oxidized flavour
Clear PET bottle 5a 4.4b 3.3b/Plastic taste 2.5c/Plastic taste, oxidized flavour 1.1b/Plastic taste, oxidized flavour
Pigmented PET bottle 5a 4.5b 3.5c 2.7c/Plastic taste, oxidized flavour 1.2b/Plastic taste, oxidized flavour
3-Layer pigmented, coextruded HDPE bottle 5a 5a 5a 4.1a 2.9a/Stale
Monolayer pigmented HDPE bottle 5a 5a 4.3b 3.4b/Slightly stale 2.9a/Stale
Coated paperboard carton 5a 5a 4.6b 3.6c/Slightly stale 3.1a/Stale, fruity
a
HDPE ¼ high-density polyethylene, PET ¼ polyethylene terephthalate. Values within a column followed by different superscript letters are
significantly different (Po0:05), asterix denotes mean of three determinations (n ¼ 3).
b
Numerical scale of scoring: very good ¼ 5, good ¼ 4, fair ¼ 3, poor ¼ 2, very poor ¼ 1, unfit for consumption ¼ 0.
 ARTICLE IN PRESS
760 A.E. Karatapanis et al. / International Dairy Journal 16 (2006) 750–761
Table 9
Concentration of dissolved oxygen (mg mL1) in whole pasteurized milk as a function of packaging material and storage time
Packaging materiala Days of storageb
1 3
Clear glass 9.170.5a
Clear PET 7.470.4b
Pigmented PET 7.370.3b
3-Layer pigmented HDPE 8.370.4c
Pigmented HDPE 7.570.3b
Coated paperboard carton 9.470.6a
a
HDPE ¼ high-density polyethylene, PET ¼ polyethylene terephthalate.
b
Values within a column followed by different superscript letters are significantly different (Po0:05). Values reported are the mean of six replicates
7SD.
pentane with storage time. The accumulation of these
compounds seems to correlate rather well with decreas-
ing flavour scores of milk (Table 7). Beginning with day
3 of storage, off-flavour notes such as ‘‘slightly stale’’
and ‘‘slightly plastic’’ were recorded in milk packaged in
containers 1, 2 and 3.
In containers that provided good protection against
light (containers 4, 5 and 6) there was a significant
increase in the concentration of ethanol, dimethyl
sulphide, ethyl acetate and a smaller increase in
concentration of esters such as methyl acetate with
increasing storage time between days 5 and 7. An
interesting observation was the formation of a series of
esters such as butyric acid methyl and ethyl ester,
hexanoic acid methyl and ethyl ester and octanoic acid
methyl ester towards the end of the milk’s shelf life.
These esters were formed in the 2 PE bottles and
particularly in the carton pack. Finally, there was an
initial increase in concentration of 2,2,4-trimethyl
pentane up to day 5 of storage which was followed by
a large decrease in this compound’s concentration on
day 7 of storage. Dimethyl disulphide, a typical product
of milk light exposure was not detected in the white/
black/white HDPE container while its concentration in
the pigmented HDPE bottle (0.6 mg L1) was 3-fold that
in the paperboard carton (0.23 mg L1). This trend in
dimethyl disulphide production is supported by spectral
transmission curves of the various packaging materials
tested (Fig. 1). Carbonyl compounds, though present in
light-protected containers, (containers 4, 5 and 6) were
found in substantially lower amounts than in light-
exposed containers (containers 1, 2 and 3). Such
compounds were formed in the light-protected contain-
ers through auto-oxidation, rather than photo-oxida-
tion, from oxygen present in the HS of the containers.
Within the storage period tested, and for the given
packaging materials, oxygen permeability (Table 8) did
not seem to significantly influence the degree of lipid
oxidation in the milk (Tables 4–6). Part of the
explanation for this may be the relatively large HS
(containing air) which was similar in all packages
5 7
8.370.5a 5.870.3a 4.370.3a
6.370.4b 5.570.5a 4.570.2a
6.970.6b 5.470.4a 3.770.2b
8.070.4a 7.570.3b 6.670.4c
7.470.5b 6.170.4a 5.670.4d
8.770.6a 8.070.5b 6.670.3c
(50–60 mL). Schröder (1982) reported that even a small
HS in a container provides a considerable O2 reservoir
relative to the quantity dissolved in milk. In a container
with a 15% HS (a common proportion for a commercial
milk carton), the ratio between dissolved and gaseous
O2 in milk at 10 1C is approximately 1:5. Thus the
contribution of dissolved oxygen in milk (Table 9) to
oxidation phenomena is rather insignificant.
No single compound is a dependable marker of the
keeping quality of milk given the relatively poor
relationship between the amount of compounds formed
(most aldehydes, sulphides, esters, hydrocarbons) and
storage time under fluorescent light. This is in agreement
with the work of Marsili (1999a) who showed a poor
correlation between the extent of light exposure,
aldehyde levels produced and perception of off-flavours
in partly defatted and skim milk.
4. Conclusion
Based on sensory evaluation, the shelf life of the Greek
whole pasteurized milk in this study was approximately 5
days. The best overall protection in terms of flavour
retention was provided by the multilayer pigmented
HDPE bottles followed by the paperboard carton and the
pigmented HDPE bottle. The onset of milk flavour
deterioration, as determined by sensory assessment,
correlated relatively well with the formation of carbonyl
compounds (hexanal, pentanal, heptanal) and dimethyl
disulphide, products of light-induced oxidation in light-
exposed containers. Correlation of sensory attributes to
levels of individual volatiles produced in the light-
protected containers was relatively poor.
Acknowledgements
The authors wish to thank the Food Certification
Unit of the University of Ioannina for providing assess
to the GC/MS instrumentation.
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