JFS:

Sensory and Nutritive Qualities of Food

Photooxidative Stability of Ice Cream

Prepared from Milk Fat
M. SHIOTA, N. IKEDA, H. KONISHI, AND T. YOSHIOKA

ABSTRACT: The photooxidation of ice cream containing 14.25% milk fat prepared from 7 fat materials with different compositions was investigated by conducting sensory evaluations for oxidized off-flavor and by monitoring
hydroperoxide formation. They showed a wide range of oxidative stability against light, and the flavor score was
related to peroxide value (correlation coefficient, 0.795). The photooxidative stability of ice cream was influenced
mainly by the riboflavin content and by the oils susceptibility to photooxidation. These contributing proportions
were 53.7 and 17.6%, respectively, with a multiple regression model. The photooxidative stability of the oil
fraction increased with the increasing tocopherol homologues ratio, g-tocopherol/a-tocopherol (correlation
coefficient,
0.846). Furthermore, the photooxidative stability of ice cream was influenced by the amount of free-fat content.
Keywords: ice cream, milk fat, b-carotene, tocopherol, photooxidative stability, riboflavin, transition metal, free fat

Introduction

CE CREAM IS A FROZEN DAIRY PRODUCT THAT IS WIDELY CONSUMED

Sen
sory
and
Nut
ritiv
e
Qua
lities
of
Foo
d

throughout the world. It contains approximately 8 to 15% fat

(Li and others 1997) because fat plays an important role in bringing the desired characteristics to ice cream: a smooth, creamy,
soft feeling in the mouth, and a good flavor (Guinard and
others
1997). Ice cream has some unique characteristics such as the solid fat network ( Thomas 1981), and these characteristics have
been studied by many researchers. Schmidt and Smith (1989) reported the effects of processing condition on the physical properties of ice cream. Goff and others (1989) studied the influence
of milk components on the physical properties of ice cream.
Ohmes and others (1998) reported sensory and physical properties of ice creams containing milk fat or fat replacers. Most of the
research on ice cream has focused on its physical characteristics
and sensory aspects.
Recently, most grocery stores have adopted stronger lighting
than ever on food products to show their products attractively.
Since the business hours in grocery stores are often extended,
the potential risk of light-induced degradation of food products
would be increased. Deterioration resulting from oxidation during storage has not been considered an important problem for
ice cream because ice cream is usually kept in frozen conditions
at 18 to 20 C (Azzara and Campbell 1992). Ice cream, however,
contains a high percentage of fat compared with other food products; therefore, ice cream might deteriorate during storage under
strong lighting in grocery stores. Light-induced oxidation could
potentially cause serious problems in the quality and safety of
ice cream.
With respect to light-induced oxidation of edible fats and oils,
several articles have been published. The oxidation strongly depends on the fatty acid composition of oil in the food products
(Cosgrove and others 1987; Neff and others 1993). Furthermore,
Dimick (1982) reported the association between the activation of
riboflavin and the degradation of dairy products. Vitamins such
as tocopherol (Parkhurst and others 1968; Cillard and others
1980; Niki and others 1984), -carotene (Matsushita and Terao
1980; Palozza and Krinsky 1992), and ascorbic acid (Cort
1974;

Miller and Aust 1989) were reported to prevent or promote the

oxidation. Light-induced oxidation of fluid milk has been well
documented and discussed in several reviews (Forss 1979; Chen
and Nawar 1991; Azzara and Campbell 1992).
However, the theories regarding light-induced oxidation of
fluid milk are considered inapplicable to the photooxidation of
ice cream because the composition (including the fat content),
manufacturing process, and storage condition of ice cream are
obviously different from that of fluid milk. Little is known about
the mechanism of light-induced oxidation of milk fat in ice
cream.
The present investigation expanded upon previous studies of
photooxidation of milk to ice cream containing 14.25% milk fat.
The objectives of the research were to determine the relation between the photooxidation of milk fat in ice cream and flavor deterioration, and to reveal the factors affecting the photooxidative
stability of ice cream. These results can help improve the photooxidative stability of ice cream.

Materials and Methods

NGREDIENTS FOR MILK FAT USED IN THIS STUDY WERE OBTAINED
FROM different commercial sources in Australia, Hungary, and

Japan. These materials were prepared with conventional

centrifugation, and the compositions are shown in Table 1.
Commercial skim milk powder (Snow Brand Milk Products Co.,
Ltd., Tokyo, Japan) was used. The following were commercially
purchased and used as ingredients for the ice cream mix:
glycerol monostearate (Rik- en Vitamin Co., Ltd., Tokyo, Japan)
as the emulsifier; mixture of locust bean gum, guar gum, and
gelatin ( Taiyo Kagaku Co., Ltd., Yokkaichi, Japan) as the
stabilizer; -carotene (Roche Holding Ltd., Basle, Switzerland)
as the coloring agent, and sugar (Dain- ippon Meiji Seito Co.,
Ltd., Tokyo, Japan). All reagents for analytical experiments were of analytical grade.

Preparation of ice cream mix

The composition of the ice cream mix is shown in Table 2.
Raw materialsskim milk,
milk-fat material, emulsifier,
stabilizer, sugar, coloring agent, and waterwere combined
as shown in

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2002 Institute of Food Technologists

Photooxidative
Photooxidative stability of ice cream . . .

Table 1Composition of milk-fat materials used for ice

cream samples (Nr 1 through Nr 7)

Table 2Ice cream formulation

ay
These of
experiments
werefor
duplicated.
od. 1949).
The scores
Nr 7 exposed
3 and 7 d were higher than

Nr The
7. contents of the tocopherol were measured by high-per-

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Content %

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Photooxidative
Photooxidative stability of ice cream . . .
Ice cream samples
Nr

Fat
%

Solids, non-fat
%

Water
%

1
2
3
4
5
6
7

40.0
68.0
78.0
75.0
69.0
60.0
84.0

4.8
2.0
4.0
1.0
4.0
10.0
1.8

55.2
30.0
18.0
24.0
27.0
30.0
14.2

Fat
Solids, non-fat
Sugar
Emulsifier
Stabilizer
Coloring agent
Water

14.25
11.50
12.76
0.25
0.20
0.06
60.98

Sensory evaluation

Ice cream production

These prepared ice cream mixes were aged overnight at 5 C,
then frozen in an ice cream freezer (APV Crepaco, Inc., Chicago,
Ill., U.S.A.) to 5 C. The overrun of all samples was 70%. These
frozen mixes were filled and packaged in 50-mL containers and
kept at 20 C.

Extraction of oil fraction from milk-fat materials

Sensory evaluations of ice cream samples exposed to fluorescent light for 0-, 3-, and 7-d intervals were conducted by 6
trained panelists. Before evaluation, a 1-h training session was
held to familiarize the panelists with the evaluation method.
During the training session, samples that contained the oxidized
off-flavor were presented to the panelists, and these panelists
were instructed to estimate the characteristic identified as oxidized off-flavors. The samples used during training evaluation
were taken from ice cream, both fresh and exposed to light for
various times to obtain different intensities of oxidized flavor. In
this session, panelists were also taught how to evaluate samples.
The trained 6 panelists evaluated the ice cream for intensity
of oxidized flavor. Ice cream samples were served at 12 C in a
50-mL capacity white paper cup. All samples were coded with
random numbers, and all orders of serving were completely randomized. The ice cream samples were served at room temperature in partitioned booths illuminated with white fluorescent
lights. Filtered water (21 C) was provided to cleanse the palate
of panelists between the samples. Panelists were instructed also
to rest between samples to avoid fatigue. The intensity of lightinduced deterioration of the samples was scored on a 10-point
scale. Scoring was from 1, very strong oxidized flavor, to 10, no flavor defected.

The milk-fat materials adopted in this study were dissolved in

n-hexane/diethyl ether (1:1, v:v) and then shaken strongly by a
vortex mixer (MT-51, Yamato Scientific Co., Tokyo, Japan) for
3 min. The upper phase was collected and the solvent was
re- moved by a roto-evaporator to obtain the oil fraction from
the milk-fat materials (REI-N, Asahi Techno Glass Corp.).
Fat

Extraction of ice cream oil part

The whole cup of ice cream samples used for each analysis
was dissolved in n-hexane/diethyl ether (1:1, v:v) and then shaken strongly by a vortex mixer for 3 min. The upper phase was collected and the solvent was removed by a roto-evaporator to obtain the oil part from ice cream samples.

Light-exposing storage test

The light-exposing storage test was carried out for the ice
cream samples and for the oil fractions: (1) The ice cream samples (50 g of each) were packed in white paper containers with
transparent polyethylene terephthalate caps. These samples
were placed on shelves exposed to 650 l x fluorescent light from
the top and kept at 20 C. At intervals of 0, 1, 2, 3, 5, and 7 d, we
removed the ice cream samples and determined the peroxide
values (PVs). The display case was illuminated by cool white fluorescent lamps mounted parallel to the shelves at a distance of
50 cm from the samples. (2) The oil fractions (10 g of each) were
kept in 7.2-cm-dia petri dishes and placed on shelves under
the same conditions. At intervals of 0, 3, and 7 d, we removed oil
frac- tion samples and determined the PVs.
Photooxidative stability was evaluated by PV determined by
the colorimetric ferric thiocyanate method (Chapman and Mack-

ay
These of
experiments
werefor
duplicated.
od. 1949).
The scores
Nr 7 exposed
3 and 7 d were higher than
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anal

ysis
The fat content of all milk-fat materials was measured by
Roese-Gottliebs method (AOAC 1991). Free-fat content, which
was regarded as fat outside the fat globules in ice cream, was
measured as described by Noda (Noda and Shiinoki 1986). The
fatty acid composition of the oil fraction was measured by gas liquid chromatography, as follows. An oil sample was transmethylated by potassium hydrate (KOH) to obtain the fatty acid methyl esters, which were dissolved in n-hexane and injected into the
gas liquid chromatograph. The fatty acid composition was measured using the following equipment: Hewlett-Packard HP6890
series II (Hewlett-Packard, Palo Alto, Calif., U.S.A.); detector,
flame-ionization detector (Hewlett-Packard); column, fused-silica capillary column, DB-WAX (30 m, 0.25 i.d., 0.25 M [film], J & W
Scientific, Folsom, Calif., U.S.A.); and carrier gas, helium.

Analysis of vitamins and minerals

The -carotene content in each oil fraction was measured by
high-performance liquid chromatography under the following
conditions: column, Shodex PSpak DS-613 (150 mm 6.0-mm
i.d., Showa Denko K.K., Tokyo, Japan); mobile phase, methanol/
n-hexane/benzene = 2:1:1; detection, UV/VIS detector (UV-970,
JASCO Corp., Hachioji, Japan) at a wavelength of 453 nm; column
oven temperature, 60 C; flow rate, 0.8 mL/min.

Nr The
7. contents of the tocopherol were measured by high-perVol. 67, Nr. 3, 2002JOURNAL OF FOOD SCIENCE

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Sensory and Nutritive Qualities of Food

the table to obtain 100 kg of mix. All mixes were prepared with fat
content set at 14.25%, and the concentration of non-fat milk solids was adjusted to 11.50% by the addition of skim milk and water. The raw materials were dissolved and mixed well in water
and pasteurized at 80 C for 60 s. The ice cream mixes were
homoge- nized at a total pressure of 150 kg/cm2 and secondary
pressure of
50 kg/cm2 by using a homogenizer (Sanwa Machine Co., Inc., Numazu, Japan).

Table 3Time dependence of flavor score of ice creams

exposed to 650 l fluorescent light at 20 C
Ice cream samples
Nr

Storage period (d)

3

0
a

1
7.67
4.50a
8.67a
6.67
6.33bc
2
3
8.67a
6.50ab
5.67abc
4
8.58a
7.00ab
5.83abc
5
8.75a
6.92ab
5.50ac
could carry over into the ice cream anda lowers the relative
con6
8.75
7.00ab
6.33bc
Values followed
same astorage period are
not bsignificantly different
7 by the same letters at 9.00
8.17
7.42atb
5.25a
ab

those of other samples. And scores of Nr 1 exposed for 3 and 7 d

were lower than those of other samples. Insignificant differences
of flavor scores were observed among samples Nr 2, 3, 4, 5, and 6.
These results indicated that milk-fat materials used for ice cream
preparation in this study led to different degrees of intensity for
photo-induced off-flavor.
The quality of ice cream depends upon the source of basic ingredients, especially milk fat. An oxidized flavor in the milk fat

sumer
acceptability
of the
ice differences
cream (AbdofEL-Rahman
others
1997). From
this report,
flavor scoresand
among
ice
cream samples stored 0 d in this study was suggested to be influenced by the differences in milk fats oxidized flavor. This result
showed the importance of the initial quality of the starting raw
formance liquid chromatography under the following conditions: materials, especially the milk fat, for the light-exposed products
column, Zorbax NH2 (250 mm 4.6-mm i.d., Hewlett-Packard, quality.
Palo Alto, Calif., U.S.A.); mobile phase, n-hexane/2-propanol = 49:1; detection, fluorescence detector (FP-920S, Jasco Milk-fat materials and light-induced oxidation
Corp., Hachioji, Japan) at a wavelength of Ex 298 nm and Em 325
The photooxidative stability of ice cream samples prepared
nm; column oven temperature, 35 C; flow rate, 1.3 mL/min.
from 7 milk-fat materials was evaluated. After the samples were
The contents of the ascorbic acid were measured by high-per- exposed to fluorescent light for storage periods of 0, 1, 2, 3, 5, and
formance liquid chromatography under the following conditions: 7 d, the oil fraction PV extracted from them was determined, as
column, Nucleosil Si100 3 m (150 mm 6.0-mm i.d., GL Sciences shown in Figure 1. These PVs increased with the increasing storInc., Tokyo, Japan); mobile phase, n-hexane/ethyl acetate/n- age period. The PV of ice cream sample Nr 1 increased signifipropanol/acetic acid = 40:30:2:1; detection, UV/VIS detector cantly faster than that of other samples, and those of samples Nr
(UV-970, JASCO Corp., Hachioji, Japan) at a wavelength of 495 6 and Nr 7 increased insignificantly. After the samples were exnm; column oven temperature, 25 C; and flow rate, 1.3 mL/min. posed to fluorescent light for the 7-d storage period, sample Nr 1
The contents of the riboflavin were measured by high-perfor- showed the highest PV, 6.8 meq/kg among the samples, and the
mance liquid chromatography under the following conditions: PVs of samples Nr 6 and Nr 7 were as low as approximately 1.3
column, Cosmosil 5 C18 (150 mm 4.6-mm i.d., Nacalai Tesque meq/kg. This result showed that ice cream could have different
Co., Ltd., Kyoto, Japan); mobile phase, 10 mM of NaH2PO4 (pH = susceptibilities on the light-induced oxidation depending on the
5.5) / methanol = 70:30; detection, fluorescence detector (F1100, fat ingredients used in this study.
Hitachi Ltd., Tokyo, Japan) at wavelengths of Ex 445 nm and Em
530 nm; column oven temperature, 40 C; and flow rate, 0.8 mL/
min.
Minerals were identified and quantified by inductively coupled plasma (ICP) emission spectrometry (ICPS-8000, Shimadzu
Corp., Ltd., Kyoto, Japan) ( JISC 1998).
P < 0.05.

Statistical analysis
Means obtained from flavor scores were subjected to analysis
of variance according to the Statistical Analysis System (SAS) (SAS
Institute 1992). The probability for statistical significance was set
at P < 0.05. The combined influence between peroxide formation
of the oil part and riboflavin content was investigated with multiple regression analysis. Prior to this analysis, the average and
standard deviation of variables were transformed to 0 and 1, respectively. This analysis was performed with SAS software.

Results and Discussion

Sensory evaluation of oxidized flavor after storage

Sen
sory
and
Nut
ritiv
e
Qua
lities
of
Foo
d

Flavor changes during the storage of ice cream samples,

which were prepared from 7 fat materials and exposed to fluorescence light, were determined by sensory evaluation. The total
amount of fat content of all ice cream samples in this study was
set to a definite percentage of 14.25% because fat content in a
food influences both texture and flavor (Li and others 1997).
Ta- ble 3 shows the results of sensory evaluation on the 7 ice
cream samples for the storage period of 0, 3, and 7 d. The flavor
Figure 1Time dependence of peroxide value of fat part
score decreased as the storage period increased. This result in ice creams exposed to 650l fluorescent light at 20 C.
indicated an increase in intensity of oxidized flavor during the Samples:
Nr 1;
Nr 2;
Nr 3;
Nr 4;
Nr 5;
Nr 6;
storage peri-

Table 4Composition of oil fraction from milk-fat materials

Fatty acid composition (%)
C4:0
C6:0
C8:0
C10:0
C12:0
C14:0
C14:1
C15:0
C16:0
C16:1
C18:0
C18:1
C18:2
C18:3
Oxidizabilitya
-Carotene ( g/100 g)
Tocopherol (mg/100 g)
-Tocopherol
-Tocopherol
-Tocopherol
-Toc./ -Toc.

Nr 1

Nr 2

Nr 3

Nr 4

Nr 5

Nr 6

Nr 7

1.9
1.5
1.0
2.4
3.0
11.1
1.0
1.3
31.9
1.5
13.2
21.5
2.0
1.6
0.0563
426

1.8
1.6
1.2
2.9
3.6
11.8
1.0
1.3
29.8
1.6
11.6
22.3
2.2
2.0
0.06646
589

1.8
1.5
1.0
2.6
3.3
10.8
1.1
1.3
31.7
2.0
10.2
23.4
3.1
1.4
0.06368
456

2.0
1.6
1.1
2.5
3.0
10.8
0.9
1.1
29.6
1.7
12.4
24.1
2.2
1.9
0.06482
474

1.5
1.4
1.1
2.6
3.2
10.5
0.9
1.1
28.7
1.8
12.6
25.6
2.5
1.9
0.06812
607

1.9
1.5
1.1
2.7
3.3
10.6
0.9
1.1
30.3
1.6
11.6
24.1
3.9
1.0
0.0638
326

1.9
1.6
1.1
2.8
3.4
11.2
1.0
1.2
31.3
1.5
11.5
22.9
3.2
1.0
0.05658
114

1.90
nd
0.01
0.0053

2.15
0.01
0.03
0.0140

3.00
0.01
0.04
0.0133

3.48
nd
0.03
0.0086

2.83
nd
0.04
0.0141

1.22
nd
0.11
0.0902

1.42
nd
0.15
0.1056

a Calculated by the following formula: 0.02 oleic acid content(%) + linoleic acid content(%) + 2 linolenic acid content(%)

nd = not detected

The relationships between flavor scores and PVs determined

for ice cream samples were estimated as shown in Figure 2. The
flavor score decreased with increasing peroxide values. And the
correlation coefficient r was 0.795 (n = 21). Photooxidation of the
oil part in milk was reported to affect flavor deterioration (Forss
1979; Azzara and Campbell 1992). The result in this study suggested that the development of off-flavor in ice cream exposed to

fluorescent light may be due to photooxidation of milk fat in ice

cream.

Photooxidative stability of oil fractions

The photooxidative stability of the oil fraction extracted from
milk-fat materials used in this study was evaluated. The PV of
the oil fraction increased with the increasing storage period as
shown in Figure 3. The PV of Nr 3 exposed 7 d was higher than
those of other samples. And the PVs of Nr 6 and Nr 7 exposed 7 d
were lower than those of other samples.

Figure 2Correlation between flavor score and peroxide Figure 3Time dependence of peroxide value of oil fracvalues of fat part in ice creams exposed to 650l fluores- tion extracted from milk-fat materials exposed to 650l
cent light at 20 C for 7 d (correlation coefficient, n = 21, fluorescent light at 20 C. Samples:
Nr 1;
Nr 2;
Nr
and
that of ice creams
r = 0.795)
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3;
Nr 4;
r = 0.367)

Nr 5;

Nr 6;

Nr 7

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Sensory and Nutritive Qualities of Food

Relationship between flavor score and generation of

hydroperoxide

Table 5Composition of hydrophilic substances of ice cream samples

Riboflavin (mg/100 g)
Ascorbic acid (mg/100 g)
Mineral (mg/100 g)
Na
K
Ca
Mg
P
Fe
Zn
Cu
Mn

Nr 1

Nr 2

Nr 3

Nr 4

Nr 5

Nr 6

Nr 7

0.0945
0.775

0.0593
0.198

0.0455
nd

0.0496
nd

0.0535
nd

0.0601
nd

0.0438
nd

8.94
27.83
17.50
1.67
16.07
0.04
0.08
nd
nd

2.96
12.61
6.11
0.70
7.37
0.04
0.05
nd
nd

1.78
7.15
2.95
0.39
4.60
0.03
0.04
nd
nd

1.93
7.06
3.64
0.43
4.59
0.04
0.05
nd
nd

1.85
6.85
3.75
0.46
5.40
0.03
0.04
nd
nd

22.38
13.10
47.58
2.40
33.32
0.06
0.21
nd
nd

1.38
4.94
2.23
0.32
4.26
0.04
0.05
nd
nd

nd = not detected

Figure 4 shows the correlation between the increased PVs

( PV ) of the ice cream oil parts and those of oil fractions exposed
for 7 d. The numbers shown on the plots indicate the sample
numbers. The PVs of these milk-fat materials oil fractions were 5
times higher than those of the corresponding ice cream samples
oil parts under this experimental condition. A high correlation of
PV was observed between milk-fat materials oil fractions and
ice cream samples oil parts for samples Nr 2, 4, 5, 6, and 7 (r =
0.935). However, samples Nr 1 and 3 did not belong to the high
correlation described above. The PV of the oil parts in ice cream
samples was relatively high compared with the oil fraction for
sample Nr 1. On the contrary, PV was relatively low in ice cream
for sample Nr 3 compared with the oil fraction. These results indicate that the photooxidative stability of ice cream depends on
the oxidative stability of its oil part, but other factors mentioned
later are affecting the photooxidative stability of ice cream.

Effect of milk-fat components

Photooxidative stability of milk has been reported to be af-

Sen
sory
and
Nut
ritiv
e
Qua
lities
of
Foo
d

Figure 4Correlation of

peroxide values of oil fractions

fected by the composition of fatty acid or vitamins in it (Cillard

and others 1980; Cosgrove and others 1987; Olsen and Ashoor
1987). These compositions are attributed to the seasonal differences in feeding conditions or processing conditions of several
milk products, and so on (Norris and others 1973; Bassette and
others 1983; Jensen and others 1999).
To investigate the factors affecting light-induced oxidation of
the oil fraction of milk-fat materials, we determined the compositions of oil fractions. As shown in Table 4, the fatty acid composition and the contents of some oil-soluble vitamins, tocopherols,
and -carotene, were determined. It is well known that the oxidative stability of saturated fatty acids > monounsaturated fatty acids > polyunsaturated fatty acids. Thus the oxidizability of these
oil fractions, which were calculated on the basis of the unsaturated fatty acid composition (Cosgrove and others 1987), was also
shown in Table 4.
Oxidizability = 0.02 oleic acid content (%) + linoleic acid content (%) + 2 linolenic acid content (%)

Figure 5Correlation between peroxide values of oil fractions and oxidizability (correlation coefficient, n = 7,

Table 6Free-fat contents and oxidizability of ice cream

samples.

quencher of activated oxygen (Matsushita and Terao 1980; Goulson and Warthesen 1999). However, the results showed that
-

cient,
n = manufacturing
7, r = 0.846) process, in which processed milk-fat
zen in the

r = 0.634).
Dutton
HJ, Schwab AW, Moser HA, Cowan JC. 1948. The flavor problem of soy-

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Ice cream samples

No
1
3
6
7

Free-fat content/
total fat content %

Oxidizability
rati o a

33.29
18.24
37.25
28.10

1.04
0.94
0.98
0.93

a Oxidizability ratio = oxidizability of free fat to oxidizability of total fat.

carotene could adversely affect and lessen the photooxidative

stability for milk fat. A more precise investigation is required to
clarify the impact of -carotene.
These results indicate that the photooxidative stability of the
oil fraction depended on the composition of the oil-soluble vitamins, such as tocopherol and -carotene; however, the influence
of fatty acid compositions on the photooxidative stability of oil
was lower under the conditions in this study.

Another factor affecting light-induced oxidationthe effect

of hydrophilic substances, such as riboflavin, ascorbic acid, and
mineralswas investigated. Transition metals like Cu and Fe
(Hegenauer and others 1979) and ascorbic acid (Parkhurst and
others 1968) were reported to involve oil autooxidation. The influence of riboflavin on light-induced fat oxidation was especially important (Korycka-Dahl and Richardson 1978; Azzara and
Campbell 1992). The compositions of these hydrophilic substances in ice cream samples are shown in Table 5. Ice cream
sample Nr 1 shows the highest riboflavin content. Oxidation that
involves riboflavin was presumed to progress in fluid milk as follows: First, riboflavin is reduced by light with the amino acid (Korycka-Dahl and Richardson 1978). Reduced riboflavin is reoxidized to form a superoxide anion. Riboflavin is capable of
generating singlet oxygen via the excited triplet state or superoxide anion. The photogeneration of singlet oxygen could lead to
autooxidation of unsaturated fatty acid (Rawls and Santen 1970).
Ice cream samples Nr 1 and 2 contained ascorbic acid, and other
samples did not contain ascorbic acid. In this experiment, the influence of ascorbic acid on the photooxidation was not clear. Ice
cream sample Nr 1 showed lower oxidative stability compared
with the correlation with PV of oil fractions, as shown in Figure

Figure 6Correlation between peroxide values of oil fractions and -tocopherol/ -tocopherol (correlation coeffi-

Figure 7Correlation between peroxide values of oil fractions and -carotene content (correlation coefficient, n = 7,

cient,
n = manufacturing
7, r = 0.846) process, in which processed milk-fat
zen in the

r = 0.634).
Dutton
HJ, Schwab AW, Moser HA, Cowan JC. 1948. The flavor problem of soy-

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Vol. 67, Nr. 3, 2002JOURNAL OF FOOD SCIENCE

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Sensory and Nutritive Qualities of Food

Hydrophilic fraction of milk-fat materials

The influence of composition differences on light-induced oxidation was examined. To compare the susceptibility of the photooxidation of the oil fraction, the increasing rate of peroxide formation from 0 to 7 d was defined as PV (oil). The correlation
coefficients between the PV (oil) of oil fractions and oxidizability, tocopherol composition, and
-carotene concentration
were determined.
The oxidizability values ranged narrowly from 0.056 to 0.068.
The PV (oil) of the oil fractions and oxidizability showed low correlation (correlation coefficient r = 0.367), as shown in Figure 5.
The effects of tocopherols composition on the PV (oil) of the oil
fractions are shown in Figure 6. The amount of tocopherols affected the photooxidative stability of the oil fraction. The PV
(oil) decreased with the increasing -tocopherol/ -tocopherol ratio with a high correlation (correlation coefficient r = 0.846). The
results showed that -tocopherol is effective in obtaining photooxidative stability for milk fat, and supported previous research
reporting that antioxidative activity of tocopherol increased
in the order of
<
<
<
(Griewahn and Daubert 1948).
Figure 7 shows the effect of -carotene content on PV (oil) of the
oil frac- tions. The
PV (oil) increased with increasing
-carotene con- tent, and the correlation coefficient (r) was 0.634.
-Carotene was
reported to inhibit lipid photooxidation because of its ability as a

4. It was suggested that riboflavin could promote photooxidation

in ice cream.
Among transition metals, Cu was known to act as a strong
prooxidant (Dutton and others 1948). However, the amount of
Cu in all ice cream samples was trace level (under 0.01 mg/100 g)
to promote milk-fat oxidation (Renner 1983). Furthermore, sample Nr 6 contained the highest amount of transition metals
among samples, had a low concentration of Fe (0.06 mg/100 g),
and did not promote photooxidation. It was inferred from this result that the content of transition metals was so low that the contribution of metals to photooxidation of ice cream appears insignificant.

Combined influence of some factors on the

photooxidation of ice cream

globules are de-emulsified and a portion of milk fat, discharged

from milk-fat globules, is present in free-fat form ( Thomas 1981).
The free-fat content of several ice cream samples in this study
was determined ( Table 6) to investigate the effect of free fat on
photooxidative stability. Ice cream sample Nr 3 showed 18.24%
free-fat content, which was lower than other ice cream samples.
Ice cream sample Nr 3 showed high oxidative stability in spite of
the low oxidative stability of the oil fraction, as shown in Figure 4.
This result indicates that free-fat content affects the photooxidative stability of ice cream and suggests that the fat in milk globules has higher photooxidative stability than the free fat in ice
cream. An insignificant difference of oxidizability, which was calculated on the basis of fatty acid composition, was observed between the oil fraction from milk-fat materials and free fat from
ice cream samples. This indicates that the de-emulsification of
the milk-fat globule to discharge free fat takes place with no
specificity on fatty acid species. These results showed that fatty
acids in free fat can be oxidized easier by light than can fatty acids in milk-fat globules, in spite of fatty acid compositions that
are the same in both free fat and globules.

The combined influence of the photooxidative stability of the

oil fraction of ice cream was investigated with multiple regression
analysis. The combined influence between oxidizability and -tocopherol/ -tocopherol on the photooxidative stability of the oil
fraction was determined. The -carotene content in milk-fat materials was dropped from the regression analysis because -carotene was added as a coloring agent in this ice cream mix, and the
Conclusions
amount of -carotene carried over from milk-fat ingredients was
HE PHOTOOXIDATIVE STABILITY OF ICE CREAM SAMPLES PREPARED
too low in comparison with that of -carotene to affect the photofrom 7 different milk-fat ingredients was investigated. We
oxidation of ice cream. Prior to the multiple regression analysis, all observed that photooxidation of ice cream affected its oxidized
data were standardized. Through the standardization process, the flavor development. The combined influence of the photooxidaaverage and standard deviations of valuables were transformed tive stability of the oil part and riboflavin content on the phototo
oxidative stability of ice cream was evaluated by multiple regres0 and 1, respectively. The multiple linear model
sion analysis. In this analysis, the susceptibility for
was:
photooxidation of the oil part ( PV [oil]) and riboflavin content
were identified and confirmed as important attributes for the
PV (oil) = 0.05 oxidizability 0.83 -tocopherol/ -tocopherol
photooxidative stability of ice cream. The susceptibility of photooxidation of the oil part was influenced by the oxidizability of fatwhere PV (oil) is the PV of the oil fraction increased during 7 d.
ty acid in the fat ingredient and tocopherol composition.
In this regression equation, the coefficient of determination (R2)
The results in this study suggested that vitamin concentration
was 0.72. Thus 72% of the variation of data was explained by the
was important to the composition of ice cream, and free-fat concombination of oxidizability and -tocopherol/ -tocopherol. The
tent in ice cream was important to structure. The fatty acid
contributing proportion of oxidizability and -tocopherol/ -tococompo- sition and the concentration of vitamins in milk fat vary
pherol on the photooxidative stability of the oil fraction was 2.0%
widely be- cause of differences in dietary intake and genetic
and 69.9%, respectively. These results indicated that the
differences between cows. These also are influenced by the
toco- pherol composition had more effect than the fatty acid
season, breed, lactation period, and other factors (Norris and
composi- tion on the photooxidative stability of oil fraction
others 1973; Hart- man and Dryden 1974; Jensen and others
extracted from milk-fat materials.
1999). This result can help improve the photooxidative stability
Next, the combined influence of the susceptibility for photoof ice cream by improv- ing the selection of ingredients and
oxidation of the oil fraction and the riboflavin concentration
preparation conditions.
was investigated with multiple regressions. The multiple linear
mod- el was:

References

PV (ice) = 0.47 PV (oil) + 0.76 riboflavin

Sen
sory
and
Nut
ritiv
e
Qua
lities
of
Foo
d

where PV (ice) is the PV of ice cream, which increased over 7 d.

In this regression equation, the coefficient of determination (R2)
was 0.71. Thus 71% of the variation of data was explained by the
combination of the PV (oil) and the riboflavin content in ice
cream. The contributing proportions of the PV (oil) and riboflavin content on the photooxidative stability of ice cream were
17.6% and 53.7%, respectively.
This result suggested that the photooxidative stability of ice
cream was influenced by the combination of riboflavin content
and the susceptibility for photooxidation of the oil fraction.

Free-fat content dependence

Ice cream has a structure in which whipped air bubbles are
stabilized by a network of solid milk fat. The ice cream mix is fro-

Abd El-Rahman AM, Shalabi SI, Hollender R, Kilara A. 1997. Effect of milk fat
fractions on the sensory evaluation of frozen desserts. J Dairy Sci 80(9):19361940.
[AOAC] Association of Official Analytical Chemists. 1991. Official method of
analysis. 16th ed. Vol. II. AOAC Official Method 920.111. Arlington, VA: Association of Official Analytical Chemists.
Azzara CD, Campbell LB. 1992. Off-flavors of dairy products. In: Charalambous
G, editor. Off-flavors in Foods and Beverages. Amsterdam: Elsevier Science
Publishers. P 329-374.
Bassete B, Fung DYC, Roberts H. 1983. Effect of pasteurization temperature on
susceptibility of milk to light-induced flavor. J Food Prot 46:416-419.
Chapman RA, Mackay K. 1949. The estimation of peroxides in fats and oils by the
ferric thiocyanate method. J Am Oil Chem Soc 26(7):360-363.
Chen ZY, Nawar WW. 1991. Role of milk fat globule membrane in autoxidation of
milk fat. J Food Sci 56(2):398-401, 426.
Cillard J, Cillard P, Cormier M. 1980. Effect of experimental factors on the prooxidant behavior of -tocopherol. J Am Oil Chem Soc 57(8):255-261.
Cort WM. 1974. Antioxidant activity of tocopherols, ascorbyl palmitate, and ascorbic acid and their mode of action. J Am Oil Chem Soc 51(7):321-325.
Cosgrove JP, Church DF, Pryor WA. 1987. The kinetics of the autoxidation of
poly- unsaturated fatty acids. Lipids 22(5):299-304.
Dimick PS. 1982. Photochemical effects on flavor and nutrients of fluid milk. Can
Inst Food Sci Technol J 15(4):247-256.

as affected by triacylglycerol composition and structure. J Am Oil Chem Soc

70(2):163-168.
Niki E, Saito T, Kawakami A, Kamiya Y. 1984. Inhibition of oxidation of methyl
linoleate in solution by vitamin E and vitamin C. J Biol Chem 259(7):41774182.
Noda M, Shiinoki Y. 1986. Microstructure and rheological behavior of whipping
cream. J Texture Stud 17:189-204.
Norris GE, Gray IK, Dolby RM. 1973. Seasonal variations in the composition and
thermal properties of New Zealand milk fat. J Dairy Res 40:311-321.
Ohmes RL, Marshall RT, Heymann H. 1998. Sensory and physical properties of
ice creams containing milk fat or fat replacers. J Dairy Sci 81(5):1222-1228.
Olsen JR, Ashoor SH. 1987. An assessment of light-induced off-flavors in retail
milk. J Dairy Sci 70(7):1362-1370.
Palozza P, Krinsky NI. 1992. -carotene and -tocopherol are synergistic antioxidants. Arch Biochem Biophys 297(1):184-187.
Parkhurst RM, Skinner WA, Sturm PA. 1968. The effect of various concentrations
of tocopherols and tocopherol mixtures on the oxidative stability of a sample
of lard. J Am Oil Chem Soc 45(10):641-642.
Rawls HR, Santen PJV. 1970. A possible role for singlet oxygen in the initiation
of fatty acid autoxidation. J Am Oil Chem Soc 47(4):121-125.
Renner E. 1983. Milk and dairy products in human nutrition. Mnchen: W-GmbH,
Volkswirtschaftlicher Verlag. p 333-338.
SAS Institute. 1992. SAS/STAT users guide. Version 6.04. Cary, N.C.: SAS Institute
Inc.
Schmidt KA, Smith DE. 1989. Effects of varying homogenization pressure on the
physical properties of vanilla ice cream. J Dairy Sci 72(2):378-384.
Thomas EL. 1981. Structure and properties of ice cream emulsions. Food Technol
35(1):41-48.
MS 20000901 Submitted 9/5/00, Accepted 11/23/01, Received 3/11/02

Authors Shiota, Ikeda, Konishi, and Yoshioka are with the Technology
and Research Institute, Snow Brand Milk Products Co., Ltd., 1-1-2
Minamidai, Kawagoe, Saitama 350-1165, Japan. Direct inquiries to
author Shiota (E- mail: m-shiota@mtf.biglobe.ne.jp).

Sensory and Nutritive Qualities of Food

bean oil. 4. Structure of compounds counteracting the effect of prooxidant

metals. J Am Oil Chem Soc 25(11):385-388.
Forss DA. 1979. Mechanisms of formation of aroma compounds in milk and milk
products. J Dairy Res 46:691-706.
Goff HD, Kinsella JE, Jordan WK. 1989. Influence of various milk protein isolates
on ice cream emulsion stability. J Dairy Sci 72(2):385-397.
Goulson MJ, Warthesen JJ. 1999. Stability and antioxidant activity of beta carotene in conventional and high oleic canola oil. J Food Sci. 64(6):996-999.
Griewahn J, Daubert BF. 1948. Delta-tocopherol as an antioxidant in lard. J Am
Oil Chem Soc 25(1):26-27.
Guinard J-X, Zoumas-Morse C, Mori L, Uatoni B, Panyam D, Kilara A. 1997. Sugar
and fat effects on sensory properties of ice cream. J Food Sci 62(5):1087-1094.
Hartman AM, Dryden LP. 1974. The vitamins in milk and milk products. In: Webb
BH, Johnson AH, Alford JA, editors. Fundamentals of dairy chemistry. Westport,
CT: Avi Publishing Company. P 325-401.
Hegenauer J, Saltman P, Ludwig D, Ripley L, Bajo P. 1979. Effect of supplemental
iron and copper on lipid oxidation in milk. 1. Comparison of metal complexes
in emulsified and homogenized milk. J Agric Food Chem 27(4):860-867.
[ JISC] Japan Industrial Standards Committee. 1998. Testing methods for
indus- trial wastewater ( JISK 0102). Tokyo: Japan Industrial Standards
Committee.
Jensen SK, Johannsen AKB, Hermansen JE. 1999. Quantitative secretion and
maximal secretion capacity of retinol, -carotene and -tocopherol into cows
milk. J Dairy Res 66:511-522.
Korycka-Dahl M, Richardson T. 1978. Photogeneration of superoxide anion in
serum of bovine milk and in model systems containing riboflavin and amino
acids. J Dairy Sci 61(4):400-407.
Li Z, Marshall R, Heymann H, Fernando L. 1997. Effect of milk fat content on
flavor perception of vanilla ice cream. J Dairy Sci 80(12):3133-3141.
Matsushita S, Terao J. 1980. Singlet oxygen-initiated photooxidation of unsaturated fatty acid esters and inhibitory effects of tocopherols and -carotene. In:
Simic MG, Karel M, editors. Autoxidation in food and biological systems. New
York: Plenum Press. P 27-44.
Miller DM, Aust SD. 1989. Studies of ascorbate-dependent, iron-catalyzed lipid
peroxidation. Arch Biochem Biophys 271(1):113-119.
Neff WE, Mounts TL, Rinsch WM, Konishi H. 1993. Photooxidation of soybean oils

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