Small Ruminant Research 125 (2015) 106114

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Small Ruminant Research

journal homepage: www.elsevier.com/locate/smallrumres

The effect of cooking time on curd composition and textural

properties of sheep Halloumi cheese
Stelios Kaminarides, Ioannis Litos, Theophilos Massouras, Aikaterini Georgala
Laboratory of Dairy Research, Department of Food Science and Human Nutrition, Agricultural University of Athens, Iera Odos 75,
11855 Votanikos, Athens, Greece

a r t i c l e

i n f o

Article history:
Received 19 February 2014
Received in revised form 29 January 2015
Accepted 30 January 2015
Available online 12 February 2015
Keywords:
Cheese curd
Sheep Halloumi cheese, Cooking time
Chemical composition
Volatile compounds
Textural properties

a b s t r a c t
The effect of cooking time on the chemical characteristics, the textural properties and the
volatile compounds of Halloumi cheese curd were studied. Sensory evaluation of the 1day Halloumi cheese was also carried out. Cooking the cheese curd for 30 min signicantly
decreased its moisture content compared to the uncooked cheese curd. The cheese curds
cooked for 30 and 60 min were found to have higher Ca and P contents in comparison with
the uncooked cheese curd. After being cooked, the cheese curds exhibited higher values for
hardness compared to the uncooked cheese curd due to their lower moisture contents.
The cooking process affected the content of most volatile compounds. Alcohols which
were found to be the main group of volatile compounds of the tested samples, consisted
85.50% of the total volatile compounds in the uncooked cheese curd and were signicantly
reduced reaching a percentage of 65.31% and 30.78% after cooking the cheese curd for 30
and 60 min, respectively. Instead, the volatile substances that were formed during thermal
processing, such as -decalactone, 3-hydroxy-butanal, 2-furan-methanol and 2-hydroxy
furanone increased signicantly. The cheese curd that was cooked for 60 min was more
yellowish in appearance compared to the cheese curd that was cooked for 30 min due to
its higher value b (yellowness). The Halloumi cheese (end product) that was produced by
cooking the cheese curd for 30 min achieved signicantly higher sensory scores than the
one that was produced by cooking the cheese curd for 60 min.
2015 Elsevier B.V. All rights reserved.

1. Introduction
Halloumi cheese is a traditional semi-hard cheese of
Cyprus and is also popular in other countries of the
Eastern Mediterranean (Papademas and Robinson, 2001).
The Committee for Standards of the Cyprus Ministry of
Commerce and Industry (1985) established the denition
and the standards for Halloumi cheese. The total exports
of Cyprus Halloumi cheese are approximately 1000 kg per

Corresponding author. Tel.: +30 2105294644; fax: +30 2105294672.

E-mail address: georgala@aua.gr (A. Georgala).
http://dx.doi.org/10.1016/j.smallrumres.2015.01.025
0921-4488/ 2015 Elsevier B.V. All rights reserved.

year (Papademas and Robinson, 2000). Initially, the milk

used for Halloumi cheese made in Cyprus was taken from
small ruminants. However, increased production of cows
milk in Cyprus has promoted the manufacture of Halloumi
cheese from cows milk alone or mixed with that of sheep
or goat. Halloumi cheese made from cows milk is more
yellowish in color and lacks the sensory characteristics
of the Halloumi cheese that is made from sheeps milk
(Kaminarides et al., 2000).
Halloumi cheese is known to have distinct sensory and
textural characteristics which result from the cooking of
the cheese curd blocks (10 cm 10 cm 3 cm) in hot nonprotein whey at 9395 C for at least 30 min, a process

S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

that does not occur in the manufacture of other cheeses

(Anifantakis and Kaminarides, 1983; Papademas and
Robinson, 2000). Cheese curd cooking destroys the rennet
and a large proportion of the microbial ora and denatures
endogenous enzymes such as alkaline phosphatase and
lipoprotein lipase (LPL), which could otherwise contribute
to the ripening of the cheese (Kaminarides and Anifantakis,
1985).
For the purpose of Halloumi cheese production from
sheeps milk two different cooking times, 30 and 60 min,
were used in order to cook the cheese curd in hot nonprotein whey at 9395 C (Anifantakis and Kaminarides,
1983) and 60 min (Galanakis et al., 2014).
The objectives of this study were to examine the effects
of the two cooking times on the chemical characteristics,
the textural properties and the volatile compounds of the
cooked cheese curds and also to test whether the sensory
characteristics of the Halloumi cheese would be affected
by increasing the amount of cooking time from 30 to
60 min at 9395 C, a process which is considered to be
less economical.

107

of Chios breed were used for our experiments. The feeding was concentrated and mainly consisted of maize, sunower, rice bran, molasse and
soybean, 74%, 7%, 5%, 6% and 3%, respectively and alfalfa hay. Fig. 1 shows
the cheese making process of the sheep Halloumi cheese. The uncooked
cheese curd was cut into blocks. Four blocks, each one consisting 250 g of
uncooked cheese curd was used as control sample (sample A). The other
blocks were divided into two subsequent parts. Thirty-eight blocks from
the rst part were cooked in non-protein hot whey at 9395 C for 30 min
(sample B), while 38 blocks from the second part were cooked in nonprotein hot whey at 9395 C for 60 min (sample C). Four cheese making
trials (replicates) were carried out.
2.2. Chemical analyses

2. Materials and methods

First, the pH of the cheese curds was measured with a pH-meter

(model 632, Metrohm, Herisau, Switzerland). Next, the total content in
solids was determined according to the International Dairy Federation
(IDF) Standard 4 (2004). Then, the content in fat was determined by the
GerberVan Gulic method (IDF Standard 222, 2008). After that, the content in ash was determined at 550 C in a mufe furnace to the point of
constant weight (IDF Standard 27, 1964). Furthermore, calcium, sodium,
potassium and magnesium contents were determined according to the
IDF Standard 119 (2007) using a Varian spectrAA-300 atomic absorption
spectrophotometer (Varian, England), while potassium and sodium were
determined by a Flame Photometer 410, Corning, England. Finally, content
in phosphorus was determined according to the spectrometric method as
it is described in the IDF Standard 42 (1990). Analyses were performed in
triplicate.

2.1. Cheese making experimental planning

2.3. Analysis of volatile compounds by GC/MS

One-hundred liters of fresh sheeps milk was taken from the experimental farm of the Agricultural University of Athens. A total of 40 sheep

An automatic balance pressure head-space apparatus (HS-40;

Perkin-Elmer Analytical Instruments, Uberlingen, Germany) connected

Raw sheep milk

Milk standardized to (5.2% fat)
Coagulation with rennet at 34 0C
Cheese curd cutting to 1cm diameter grains
Rest for 10 minutes
Gentle stirring for 10 minutes
Scalding up to 40 0C within 15 minutes
Transfer of the cheese curd to the hoops
Cheese curd

Whey

Pressure of 3kg/kg to
the cheese curd for 35 minutes
Cutting of the curd to pieces of 10x10x3cm
(Sample A)
Heating to 90-920C (about 30 minutes)
Remove of the whey proteins

Transfer the cheese curd pieces into the hot whey (90-92 0C )
Cooking of the cheese curd pieces

At 93-95 0C for 30 minutes (Sample B)

At 93-950C for 60 minutes (Sample C)

Drainage of the cheese curd cooked pieces on a cheese table

Addition of salt with grated dried Mentha viridis leaves
Halloumi cheese product (packing in plastic bags)

Fig. 1. Cheese making process of sheep Halloumi cheese.

108

S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

to a gas chromatographmass spectrometer (GC/MS-QP 5050; Shimadzu

Co, Kyoto, Japan) was used for the analysis of volatile compounds as
described by Kaminarides et al. (2007). Briey, 10 g of cheese samples
were homogenized in an analytical grinder (IKA, Labortechnik, Staufen,
Germany), with 20 g of Na2 SO4 and 50 L of an aqueous solution containing 0.5 mg/mL of methyl isobutyl ketone as internal standard. An aliquot
(5 g) of the mixture was introduced into 22 ml vials, which were then
sealed with aluminumrubber septa and held at 65 C for 30 min purged
and pressurized with helium at a ow rate of 35 ml/min. Samples were
analyzed in duplicate. The procedure and the identication of volatile
compounds were detected by using selected ions. Semi-quantication
was carried out by summarizing the abundance of characteristic ions
with reference to the methyl isobutyl ketone peak which was used as an
internal standard. Relative abundances of compounds were expressed in
percentages in terms of their peak areas based on the internal standard
methyl isobutyl ketone peak area.
2.4. Textural evaluation
The textural properties of the cheese curds were measured with a
Shimatzu testing instrument (model AGS-500NG, Shimatzu Corporation,
Japan) equipped with a 5-kg load cell which was used to perform the
texture prole analysis (TPA) of the cheese curds. A plunger with a diameter of 20 mm was attached to the moving crosshead. The speed of the
crosshead was set at 2.5 cm min1 in both upward and downward directions. The cheese curd sample was placed on a at holding plate at 20 C
and the plunger was inserted 20 mm below the cheese curd surface. Two
consecutive bites were taken. The following four textural characteristics
were calculated from the typical texture prole curve (Kaminarides and
Stachtiaris, 2000).
2.5. Color values
The Hunter color values L, a and b were determined by using the colorimeter Minolta CR 200 model, Osaka, Japan (Ergonul et al., 2011). Value
L represents the lightness of the color, value a represents the position
of the color between green and red and value b represents the position
of the color between blue and yellow. Ten different measurements were
performed for each sample.
2.6. Sensory evaluation
The Halloumi cheese sensory characteristics were evaluated by a
thirteen-member panel from the Dairy Laboratory of the Agricultural University of Athens. Members of the panel, who were familiar with Halloumi
cheese, evaluated each cheese sample for its appearance, texture and avor (odor and taste) on a 10-point scale, from one signifying the worst
to ten signifying the best quality. The attributes of avor and texture
were given priority over appearance, as prescribed by the IDF Standard
(1987), multiplying their scores by 5 and 4 respectively. The total score
was obtained by adding the scores based on the three attributes. An excellent cheese would receive a total score of 100 points. The results are
expressed in terms of a mean score by the whole panel for each cheese.

2.7. Statistical analysis

Statistical analysis was performed by using the general linear model
(proc GLM) statistical program S.A.S. (SAS Institute, 2005), with independent variable the cooking time of the cheese curd. The level of signicance
was xed to P = 0.05. The comparisons of means were made with the Duncan method. The results are presented as means standard error of mean.

3. Results and discussion

3.1. Chemical characteristics
The results on the chemical characteristics of the
uncooked cheese curd and of the cheese curd that was
cooked in hot non-protein whey at 9395 C for 30 and
60 min are shown in Table 1. However, cooking the cheese
curd for 30 min signicantly (P < 0.05) reduced (approximately ten centesimal units) its moisture content (Table 1).
This was attributed to the fact that water was transferred
from the cheese curd to the whey. Afterwards, an extra
30 min cooking of the cheese curd for another did not
markedly (P > 0.05) affect its moisture content (Table 1).
This possibly occurred since the creation of a surface crust
caused by the dehydration of the cheese curd limited, at a
signicant rate, the expulsion of moisture.
Cheese is known to be an important dietary source of
several minerals, in particular calcium, phosphorus and
magnesium. The mineral content of cheeses depends upon
a cheese variety and its production process. According to
Holland et al. (1995) and Economides (2004), Halloumi
cheese is considered to be a rich source of calcium, approximately 700794 mg 100 g1 . This can be compared with
the calcium level that is found in other semi-hard cheeses
such as Edam and Gouda cheeses, 770795 mg 100 g1
and 740773 mg 100 g1 , respectively. Also, the magnesium content of Halloumi cheese was found to be
3040 mg 100 g1 (Holland et al., 1995; Economides, 2004).
The magnesium contents of Edam and Gouda cheeses
were similar to that of Halloumi cheese; 39 mg 100 g1
and 38 mg 100 g1 , respectively (Holland et al., 1995). An
increase of Ca and P contents was observed from the
uncooked cheese curd to the cheese curd that was cooked
for 30 min and then in the cheese curd that was cooked for
60 min (Table 1). This explains the extraction of moisture
from the cheese curd during its cooking which resulted in

Table 1
Chemical characteristics of the Halloumi cheese curds.
Chemical characteristics

Cheese curds
A

pH
Moisture (g 100 g1 )
Fat in DM (g 100 g1 )
Ash (g 100 g1 )
Ca (mg 100 g1 )
Mg (mg 100 g1 )
K (mg 100 g1 )
Na (mg 100 g1 )
P (mg 100 g1 )

6.11
54.18a
57.86
2.32
785.5a
52.0
69.5
64.0
415.0a

0.09
0.99
0.85
0.05
14.5
0.6
11.9
20.7
15.6

6.25
44.9b
55.78
2.57
845.0b
54.3
75.8
63.5
522.5b

0.06
1.65
2.22
0.12
17.1
2.0
6.3
20.2
31.5

Values are means standard errors.

Means within each row without a superscript or bearing a common superscript did not differ signicantly (P > 0.05).
DM: dry matter. A: uncooked cheese curd; B: cheese curd cooked for 30 min, C: cheese curd cooked for 60 min.

6.29
43.03b
54.50
2.64
888.3b
56.0
69.5
65.5
545.0b

0.06
1.02
1.75
0.13
19.1
2.3
6.8
17.0
37.1

S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

109

Table 2
Relative abundance of volatile compounds isolated from the Halloumi cheese curds.
Cheese curds
A
Alcohols
Ethanol
3-Methyl-1-butanol
2-Methyl-1-propanol
1-Butanol
2-Methyl-1-butanol
1-Pentanol
Heptanol
2-Pentanol
Isopropyl alcohol
Methyl alcohol
3-Methyl, 2-butanol
Total alcohols
Percentage (%)
Ketones
2-Butanone
Acetone
3-Methyl-2-butanone
3-Hydroxy-2-butanone (acetoin)
1-Hydroxy-2-butanone
2,3-Butanedione (diacetyl)
1-Methoxy-2-propanone
Total ketones
Percentage (%)
Lactones
-Decalactone
Percentage (%)
Volatile acids
Acetic acid
Formic acid
Butanoic acid
Hexanoic acid
Total acids
Percentage (%)
Esters
Acetic acid ethyl ester
Propanic acid 2-propenyl ester
Propanic ethyl ester
Propanic pentyl ester
Acetic acid 2-propenyl ester
Formic ethyl ester
Formic-2-propenyl ester
Total esters
Percentage (%)
Aldehydes
Acetaldehyde
2-Methyl-propanal
Pentanal
Propanal
3-Hydroxy-butanal
Total aldehydes
Percentage (%)
Furans
2,5-Dihydro-furan
3-Methyl furanone
2-Furanmenthol
2-Hydroxy furanone
Total furans
Percentage (%)
Hydrocarbons
Hexadecane
Octane
2,3-Dimethyl-oct-1-en
1-Methoxy-2-decane
Butane
Heptane
2,2-Dimethyl pentane

530.52a
12.80a
20.34a
0.74a
0.41
2.76a
0.78a
0.67
0.41a
2.08a
0.34
571.85a
85.50
5.15a
6.93a
11.68a
10.70a
0.61a
2.41a
0.0a
37.58a
5.60

123.42
1.40
3.18
0.19
0.10
0.54
0.19
0.23
0.10
0.11
0.04
126.89

38.54b
2.19b
0.61b
0.23b
0.24
0.21b
0.21b
0.43
0.0b
0.52b
0.30
43.48b
65.31

10.58
0.86
0.23
0.03
0.05
0.05
0.07
0.20
0.0
0.12
0.08
11.26

2.74b
0.15b
0.0b
0.0b
0.20
0.0b
0.12b
0.22
0.0b
0.06c
0.33
3.82b
30.78

0.70
0.03
0.0
0.0
0.04
0.0
0.05
0.04
0.0
0.03
0.11
0.69

0.38
0.90
2.59
1.02
0.18
0.18
0.0
1.71

0.86b
3.00b
1.58b
2.09b
0.31a,b
2.50a
0.83b
11.59b
16.78

0.17
0.74
0.21
0.33
0.03
0.37
0.28
0.59

0.0c
2.09b
0.12b
0.21b
0.0b
0.21b
0.18a
3.76c
22.64

0.0
0.36
0.04
0.1
0.0
0.03
0.08
0.30

0.10a 0.04
0.02

0.42b 0.09
0.63

0.95c 0.14
7.66

41.87a
0.62a
4.06a
2.37a
48.92a
7.32

8.57
0.08
0.84
0.30
8.17

3.02b
0.21b
0.98b
0.74b
4.95b
7.44

0.23
0.04
0.14
0.14
0.36

0.13b
0.17b
0.18b
0.18b
0.66b
5.31

0.04
0.03
0.03
0.07
0.07

0.54a
0.71
2.27a
0.30a
0.56
0.24
0.0a
4.62a
0.69

0.03
0.43
0.73
0.03
0.23
0.03
0.0
0.88

0.34b
0.15
0.88a,b
0.09b
0.51
0.17
0.25b
2.39b
3.59

0.04
0.01
0.47
0.04
0.24
0.01
0.04
0.60

0.0c
0.16
0.0b
0.0b
0.14
0.21
0.13C
0.64b
5.16

0.0
0.02
0.0
0.0
0.01
0.04
0.03
0.05

2.91a
0.29a
0.10a
0.16
0.0a
3.46a
0.52

0.38
0.05
0.02
0.06
0.0
0.40

0.26b
0.13b
0.19a,b
0.14
0.20b
0.92b
1.38

0.06
0.04
0.03
0.05
0.04
0.04

0.0b
0.0c
0.31b
0.15
0.32c
0.78b
6.29

0.0
0.0
0.07
0.05
0.04
0.09

0.12a
0.11a
0.00a
0.00a
0.24a
0.04

0.02
0.05
0.00
0.00
0.05

0.16a,b
0.26a,b
0.13 b
0.14a
0.73b
1.10

0.02
0.07
0.02
0.05
0.01

0.54b
0.35b
0.26c
0.38b
1.34c
10.80

0.09
0.07
0.03
0.06
0.11

0.08
0.22
0.05
0.04
0.03
0.21
0.03

0.47
0.38
0.25
0.12a,b
0.13a
0.38a,b
0.82b

0.15
0.15
0.09
0.05
0.03
0.10
0.21

0.65
0.18
0.17
0.10b
0.00b
0.14b
0.16a

0.18
0.06
0.03
0.03
0.00
0.03
0.03

0.24
0.45
0.23
0.23a
0.19a
0.55a
0.27a

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S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

Table 2 (Continued)
Cheese curds
A
Total hydrocarbons
Percentage (%)

2.09a,b 0.05
0.31

2.51a 0.48
3.77

1.41b 0.11
11.36

Values (mg/kg) are means standard errors, expressed as relative abundance to internal standard.
Means within each row without a superscript or bearing a common superscript did not differ signicantly (P > 0.05).
A: uncooked cheese curd; B: cheese curd cooked for 30 min; C: cheese curd cooked for 60 min.
Percentage (%): percentage of volatile compounds of each chemical group in each of the examined cheese curds.

an increase of undissolved constituents. The milk casein

micelles are known to contain 65% undissolved colloidal
calcium phosphate. Consequently, there was an increase
of Ca and P contents during cheese curd cooking of as these
elements could not be extracted from the whey (Walstra
and Jenness, 1984; Gaucheron, 2005).
Most cheeses provide good amounts of phosphorous
although its content differs among cheese varieties. Levels of calcium and phosphorus are generally higher in hard
and semi-hard cheeses such as Parmigiano, Gouda, Edam
and Cheddar and lower in mold cheeses such as Brie and
Stilton (Holland et al., 1995). The lowest values are found
in cream and cottage type cheeses. The phosphorous content in Halloumi cheese was found to be 4445 mg 100 g1
(Economides, 2004) while the phosphorous contents of
Edam cheese and Gouda cheese were 530 mg 100 g1 and
490 mg 100 g1 , respectively (Holland et al., 1995).
Sodium levels in cheeses depend on the amount of salt
that is added during the cheese making process. The salt
content of natural cheeses is known to be lower than that of
many processed cheeses. Sodium is mainly found in cheese
whey as it is water soluble. The cheese curd samples in the
present study were low in sodium content as there was not
any added salt (Table 1).
3.2. Volatile compounds
Head space extraction coupled with GCMS allowed
the separation and identication of volatile compounds
that belong to the following chemical groups: alcohols,
ketones, volatile acids, esters, aldehydes, hydrocarbons,
and furans. Table 2 summarizes the mean for 28 quantied volatile compounds in the headspace prole before and
after Halloumi cheese curd cooking at 9395 C for 30 or
60 min. Most of the volatile compounds have been previously reported in Halloumi and whey cheeses (Kaminarides
et al., 2007, 2009). These compounds could arise not only
from the natural microbial ora of milk but also from the
whey that is heated during the manufacturing process of
Halloumi cheese. Whey contains high concentrations of
lactose, which make it highly susceptible to Maillard reaction (De Block et al., 2003).
Eleven different alcohols were detected (Table 2) and
found to be the main group of volatile compounds of the
tested samples. A high amount of ethanol was found in the
uncooked cheese curd due to the fact that native microbial ora is present in the cheese curd and as a result it
forms large amounts of ethanol through lactose fermentation (Ortigosa et al., 2001). Although ethanol is found in
high concentrations in many cheeses, it may contribute

little or not at all to the aroma of the cheese. However,

high amounts of ethanol lead to the formation of many
ethyl esters. Kaminarides et al. (2007, 2009) found that
ethanol was the principal aromatic compound of Halloumi
cheese and Halloumi-type cheese, respectively. Ethanol
is the main volatile aromatic compound produced during cheese ripening, as it has been observed in many
cheese types (Kaminarides et al., 2007; Kondyli et al., 2003).
Ethanol is produced by fermentation of lactose by hetero
fermentative lactic acid bacteria or yeasts, or by amino
acid metabolism and by acetaldehyde reduction (Munoz
et al., 2003). Due to high concentrations in ethanol, alcohols
consisted 85.50% of the total volatile compounds that were
found in the uncooked cheese curd. After having cooked
the cheese curd for 30 and 60 min the percentage (%) of
alcohols was reduced to 65.31% and 30.78%, respectively.
Apart from ethanol, 3-methyl-1-butanol and 2-methyl1-propanol were also found in high concentrations in the
uncooked cheese curd (Table 2). The amounts of ethanol
and 3-methyl-1-butanol were signicantly reduced after
cooking the cheese curd. 2-Methyl-1-propanol was not
detected in the cheese curd that was cooked for 60 min. The
other detected alcohols were found in low concentrations.
Consequently, the cooking process affected the levels of
alcohols in the cheese curd, which was heated at 9395 C
for 30 and 60 min, signicantly with the exception of 2methyl-1-butanol, 3-methyl-2-butanol and 2-pentanol.
A total of eight ketones were isolated and detected
by the head space fraction of the examined samples
and consisted 5.62% of the total volatile compounds of
the uncooked cheese curd. In the cheese curds that
were cooked for 30 or 60 min ketones consisted 17.41%
and 30.30% of the total volatile compounds, respectively.
Ketones are present in the majority of dairy products
(Engels et al., 1997). They have low perception thresholds
and are known to contribute to the cheese aroma. In the
present study, 3-methyl-2-butanone represents the most
abundant ketone found in the uncooked curd, followed by
3-hydroxy-2-butanone (acetoin), acetone and 2-butanone.
However, 3-methyl-2-butanone was signicantly reduced
in the cheese curds that were cooked in hot non-protein
whey at 9395 C for 30 or 60 min.
Acetone was also found in the uncooked cheese curd
but its content was signicantly reduced after cooking
the cheese curd for 30 or 60 min. 3-Hydroxy-2-butanone
(acetoin) was found in high amounts in the uncooked
cheese curd but it was signicantly reduced after cooking
the cheese curd at 9395 C for 30 or 60 min. The 3hydroxy-2-butanone is produced by the apocarboxylation
of a-keto-lactic acid or by the reduction of diacetyl (Izco and

S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

111

Table 3
Textural properties of the Halloumi cheese curds.
Textural properties

Cheese curds

Hardness (N)
Cohesiveness (N mm)
Adhesiveness (N mm)
Elasticity (mm)

5.05a
0.46
8.47a
0.96

0.78
0.02
0.50
0.01

7.10b
0.48
15.40b
0.97

0.51
0.02
0.44
0.01

9.98c
0.47
10.53c
0.89

0.38
0.02
0.76
0.04

Values are means standard errors. Means within each row without a superscript did not differ signicantly (P > 0.05).
A: uncooked cheese curd; B: cheese curd cooked for 30 min; C: cheese curd cooked for 60 min.

Torre, 2000; McSweeney and Sousa, 2000). Although the

amount of diacetyl was almost stable from the uncooked
cheese curd to the cheese curd that was cooked in hot
non-protein whey for 30 min, nevertheless it was significantly reduced after cooking the cheese curd for 60 min
(Table 2). Diacetyl is known to be produced mainly by
citrate metabolism (McSweeney and Sousa, 2000), has a
buttery, nut-like avor (Kondyli et al., 2003) and is more
volatile than 3-hydroxy-2-butanone (acetoin). 2-Butanone
was found in the uncooked cheese curd and was significantly reduced in the cheese curd that was cooked for
30 min. This ketone was not detected in the cheese curd
cooked for 60 min. According to Arora et al. (1995) the
aforementioned ketone is known to have a buttery avor
and is one of the major volatile compounds of Cheddar
cheese.
In this study, one lactone was detected. -Decalactone
was detected in all cheese curds and was signicant
increased after cooking the curd. This lactone is considered to be a potent dairy avor compound in butter
and buttermilk (McGorrin, 2001) and is generally used
in combination with free fatty acids (FFA) and methyl
ketones to produce creamy fatty notes in commercial avorants. Lactones contribute to cheese avor giving fruity
and sweet creamy fermented notes (Dufosse et al., 1994).
Parlimnet et al. (1966) concluded that the precursors for
lactones were triglycerides that contain a hydroxyl acid
moiety.
A total of four short chains (C6) carboxylic acids that
were isolated and detected in the head space fraction of
the examined samples, consisted 7.32% of the total volatile
compounds of the uncooked cheese curd, 7.44% of the
cheese curd that was cooked for 30 min and 5.31% of the
cheese curd that was cooked for 60 min. Even though the
amount of total acids was signicantly reduced in the
uncooked cheese curd compared to the cheese curd that
was cooked for 30 min, there was not any further significant reduction in total acids of the cheese curd that was
cooked for 60 min.
Acetic acid, formic acid, butanoic acid and hexanoic acid
were the only acids detected in our study. Butanoic and
hexanoic were found to have the same decreasing trend
during the heat treatment process of the cheese curd at 30
and 60 min. Acetic acid was the main volatile acid found
in the uncooked cheese curd. This acid was signicantly
reduced after cooking the cheese curd at 9395 C for 30
and 60 min. Acetic acid is produced by citrate or lactate
fermentation process or by amino acid catabolism from
bacteria with a harsh but not rancid avor and a typical

aroma (Barbieri et al., 1994; McSweeney and Sousa, 2000;

Munoz et al., 2003). According to Panari (1986), the concentration of acetic acid in Cheddar, Provolone, Blue Emmental,
Fontina, Sbrinz and Ossolano cheeses ranged from 0.13 to
2.96 mg/g cheese. Various short-chain volatile acids could
be important to the aroma of liquid whey (Whetstine et al.,
2003). Kaminarides et al. (2007) found high amounts of
acetic acid that range from 72 to 360 mg/kg in the 1and 45-day-old Halloumi cheese, respectively. Also a high
concentration of acetic acid (913 mg/kg) was found by
Kaminarides et al. (2009) in a 30-day-old Halloumi-type
cheese.
Seven esters detected in the present study consisted
0.69% of the total volatile compounds of the uncooked
cheese curd, 3.59% of the total volatile compounds of the
cheese curd cooked for 30 min and 5.16% of the total volatile
compounds of the cheese curd cooked for 60 min. Esters
are important because rst they owe their avor to the
high volatility at ambient temperatures and second due to
their low perception thresholds. Esters can be formed by
direct esterication of alcohols and carboxylic acids or by
alcoholysis (McSweeney and Sousa, 2000; Ortigosa et al.,
2001). Propanic ethyl ester was the most prevalent in the
uncooked cheese curd. Small amounts of acetic acid ethyl
ester and propanic pentyl ester were found in the uncooked
cheese curd and in the cheese curd that was cooked for
30 min. Nevertheless, these esters were not detected in the
cheese curd that was cooked for 60 min. Ethyl esters are
known to contribute to the development of the fruity character of cheeses. Small quantities of acetic and propanic
acid 2-propenyl ester were only found in the examined
cheese curds with no signicant differences among the
uncooked cheese curd and the cheese curds that were
cooked for 30 or 60 min. Kaminarides et al. (2009) also
found these types of esters in Halloumi-type cheese samples.
Regarding the amount of total esters, it was signicantly reduced in the uncooked cheese curd compared to
the cheese curd that was cooked for 30 min, while there
was not any signicant change in the cheese curd that was
cooked from 30 to 60 min.
Five aldehydes (acetaldehyde, 2-methyl-1-propanal,
pentanal, propanal and 3-hydroxy-butanal) were detected.
They were found in relatively small quantities. Aldehydes
consisted 0.52% of the total volatile compounds in the
uncooked cheese curd and 1.38% of the total volatile compounds in the cheese curd that was cooked for 30 min.
Aldehydes consisted 6.29% of total volatile compounds in
the cheese curd that was cooked for 60 min.

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S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

Low molecular weight aldehydes have low aroma

thresholds (Kinsella et al., 1967; Rychlik et al., 1998) and
therefore contribute to the cheeses avor. Saturated aldehydes such as pentanal are likely to originate from lipid
oxidation (Kondyli et al., 2003) and have been associated
with cardboard, fatty and unclean avors in dairy products (Tomaino et al., 2001). They are mainly produced by
amino acid catabolism or by decarboxylation of keto acids.
Since aldehydes can be either converted to their corresponding alcohols or oxidized to their corresponding acids,
only low amounts of aldehydes are expected to be found
in cheeses (Munoz et al., 2003). Low relative amounts of
acetaldehyde (2.91 mg/kg) were found in the uncooked
cheese curd. Acetaldehyde was signicantly reduced in
the cheese curd that was cooked for 30 min, while there
was no acetaldehyde detected in the cheese curd that
was cooked for 60 min. This compound was probably lost
during the above procedure due to its low boiling point
(bp 20.8 C).
Acetaldehyde is commonly detected in fermented dairy
products and has a distinct sweet and pungent smell. It is
formed by lactose metabolism, by lactic acid bacteria and
can also be produced by reversible pathways through the
action of the enzyme threonine aldolase on the amino acid
threonine (Barbieri et al., 1994; Milo and Reineccius, 1997).
Acetaldehyde was found in the 45-day-old Halloumi and
Halloumi-type cheese (Kaminarides et al., 2007, 2009).
Saturated aldehydes as pentanal and propanal that are
likely to originate from lipid oxidation (Morr and Ha, 1991)
were found in small amounts in all of the examined cheese
curd samples. Their relative abundance ranged from 0.10 to
0.31 mg/kg. These aldehydes are known to be characterized
by a green-grass and herbaceous aroma.
Reference data showed that pentanal was found in the
1-day-old Halloumi cheese (Kaminarides et al., 2007) and
in a 1- and 30-day-old Halloumi-type cheese (Kaminarides
et al., 2009). Kondyli et al. (2002) detected pentanal in
a 180-day-old feta cheese. Also, 3-hydroxy-butanal was
found only in the Halloumi cheese curd that was cooked for
30 or 60 min. Kaminarides et al. (2007) found the presence
of 3-hydroxy-butanal in a 1-, 15- and 30-day-old Halloumi
cheese, while Kaminarides et al. (2009) found 3-hydroxybutanal only in a 30-day-old Halloumi-type cheese.
In our study, four furans were detected in very low
amounts. Furans were mainly found in the cheese curds
that were cooked for 30 and 60 min and consisted 0.04% of
the total volatile compounds found in the uncooked cheese
curd, 1.10% of the total volatile compounds found in the
cheese curd cooked for 30 min and 10.80% of and the total
volatile compounds found in the cheese curd cooked for
60 min. They are widely used as avoring agents in the food
and beverage industry (Blank and Fay, 1996) due to their
pleasant taste and odor. However, little is known about the
inuence of furans on cheese avor. Furans may be generated from decarboxylation, cyclization, and dehydration of
ascorbic acid or from lipid oxidation (Perez and Yaylayan,
2004). However, they are also associated with Maillard
reactions between reducing sugars and amino acids such
as lactose and casein (Blank, 2009). There is evidence that
these compounds may contribute to the sensory properties
of some cheese varieties.

2-Furanmenthol and 2-hydroxy furanone were not

detected in the uncooked cheese curd. 2-Furanmenthol
content signicantly increased starting from the uncooked
cheese curd to the cheese curd that was cooked for 30 min
and then to the cheese curd cooked for 60 min, while there
was not any signicant change of 2-hydroxy furanone content between the uncooked cheese curd and the cheese
curd cooked for 30 min. However, this furane was signicantly increased when the cheese curd cooked from 30 min
to 60 min. Total furans content was signicantly increased
from the uncooked cheese curd to the cheese curd that was
cooked for 30 and 60 min.
Seven hydrocarbons were detected in the present study.
They consisted 0.31% of the total volatile compounds in
the uncooked cheese curd, 3.77% of the total volatile compounds in the cheese curd that was cooked for 30 min and
11.36% of the total volatile compounds in the cheese curd
that was cooked for 60 min. Hydrocarbons are secondary
products of lipid auto oxidation. Although they do not contribute to cheese aroma they may act as precursors for the
formation of other aromatic compounds (Ortigosa et al.,
2001; Munoz et al., 2003). Hydrocarbons have been frequently detected in many cheese varieties although they
are usually found at low concentrations (Carbonell et al.,
2002a,b). Kaminarides et al. (2009) found hydrocarbon
pentane to be present only in 30- and 45-day-old Halloumitype cheeses.
In the present study, small quantities of hydrocarbons
were detected. No signicant changes in the amounts of
the hydrocarbons hexadecane, octane and 2,3-dimethyloct-1-en were found from the uncooked cheese curd to the
cheese curds that were cooked for 30 or 60 min. The amount
of 2,2-dimethyl pentane was signicantly increased from
the uncooked cheese curd to the cheese curd that was
cooked for 30 min. Thereafter, this hydrocarbon was signicantly decreased to the cheese curd that was cooked
for 60 min. So, the amount of 2,2-dimethyl pentane in
the cheese curd that was cooked for 60 min did not differ signicantly from the amount that was found in the
uncooked cheese curd. Kaminarides et al. (2009) found the
hydrocarbon pentane to be present only in 30- and 45-dayold Halloumi-type cheeses. No signicant difference in the
amount of the hydrocarbon butane was found between the
uncooked cheese curd and the cheese curd that was cooked
for 30 min. However, this hydrocarbon was signicantly
reduced in the cheese curd that was cooked for 60 min.
The amounts of hydrocarbons 1-methoxy-2-decane and
heptane were reduced during the cooking process of the
cheese curd. The amounts of these hydrocarbons were
markedly lowered in the cheese curd that was cooked for
60 min than in the uncooked cheese curd (Table 2).
3.3. Textural assessment
The results on the textural characteristics are presented in Table 4. After being cooked, the cheese curds
exhibited higher values of hardness compared to the
uncooked cheese curd due to their lower moisture contents
(Tables 2 and 3). The highest value of hardness was found in
the Halloumi cheese curd that was cooked for 60 min (sample C). The lowest value for adhesiveness was found in the

S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

Table 4
Color parameters (L, a, b) of the Halloumi cheese curds.
Color values

L
a
b

Cheese curds
A

92.59a 0.11
2.76a 0.03
11.33a 0.16

91.58b 0.14
5.88b 0.07
16.10b 0.24

90.48c 0.23
5.84b 0.07
17.05c 0.32

Values are means standard errors.

Means within each row bearing a common superscript did not differ signicantly (P > 0.05).
A: uncooked cheese curd; B: cheese curd cooked for 30 min; C: cheese
curd cooked for 60 min.

fresh Halloumi cheese curd (sample A). However, the elasticity and cohesiveness values did not differ signicantly
(P > 0.5) among the cheese curds that were tested (samples
A, B and C).
3.4. Color
The Hunter color values are shown in Table 4. As far
as the lightness (L) value among the cheese curds is concerned, there were signicant differences: the uncooked
cheese curd exhibited the highest lightness value and the
cheese curd that was cooked for 60 min exhibited the lowest. The cheese curd that was cooked for 60 min was more
yellowish in appearance compared to the cheese curd that
was cooked for 30 min as its value b (yellowness of the sample) was signicantly higher than the value of the cheese
curd that was cooked for 30 min (Table 4). The application of high temperatures (9395 C) during the cheese
curd cooking, especially in the case of the cheese curd
that was cooked for more than 30 min (sample C that was
cooked for 60 min) resulted in the formation of compounds
that darken the color of the cheese curd. The formation of
these compounds is realized through Maillard reaction as
the lactose of the cheese curd reacts with its amino compounds and results in the formation of compounds that
darken the color of the cheese curd. Concerning a value
(redness of the sample) no signicant differences were
observed between the cheese curd that was cooked for
30 min and the cheese curd that was cooked for 60 min
(Table 4).
4. Sensory characteristics
The sensory characteristics of the Halloumi cheeses
were shown in Table 5. Sensory evaluation was done in

113

the 1-day-old Halloumi cheese. The Halloumi cheese that

was produced by the cheese curd that was cooked for
30 min received signicantly (P < 0.05) higher scores for
appearance, texture, avor and total sensory characteristics compared to the Halloumi cheese that was produced
by the cheese curd that was cooked for 60 min (Table 5).
When the cooking time of the cheese curd exceeds 30 min
it seems to downgrade the sensory scores of the Halloumi
cheese (Table 5).
5. Conclusion
The results of the present study showed that cooking
the cheese curd for 30 or 60 min in hot non-protein whey at
9395 C signicantly decreased its moisture content and
increased the Ca and P contents of the cooked cheese curds
as compared with the uncooked cheese curd. Although
alcohols remained to be the major group of volatile compounds they were signicantly reduced from the uncooked
to the cooked cheese curds. Similarly, other volatile substances which were detected in the uncooked cheese
curd such as methanol, 2-butanone, diacetyl, 1-methoxy2-propanone, acetic acid, the formic-2-propenyl esters,
2-methyl propanal, and the hydrocarbons butane and 2,2dimethyl pentane, were substantially reduced during the
thermal process. Also, the cooked cheese curds had higher
values for hardness compared to the uncooked cheese curd
due to their lower moisture values. The highest value of
hardness was found in the cheese curd that was cooked
for 60 min. Also, the cheese curd that was cooked for
60 min was found to be more yellowish in appearance than
the cheese curd that was cooked for 30 min. The sensory
evaluation showed that the cheese made by the cheese
curd cooked for 30 min gained signicantly higher sensory scores in comparison with the cheese made by the
cheese curd cooked for 60 min. In conclusion, the present
study showed that the most effecting time for cheese curd
cooking is 30 min, during which the products pasteurization and hygienic is ensured, since the extra 30 min cooking
resulted in an additional loss of volatile compounds, the
creation of a harder cheese curd and the formation of compounds that darken the cheese curd color and reduce the
organoleptic properties of Halloumi cheese. Therefore, we
propose cheese curd cooking at 9395 C for 30 min as it
not only reduces cheese making time and cost but it also
gains higher sensory scores for the end product (Halloumi
cheese).
Conict of interest

Table 5
Sensory characteristics of the Halloumi cheese (end product).
Sensory characteristics

Halloumi I

Appearance (110)
Texture (140)
Flavor (150)
Total (1100)

9.31a
34.15a
43.46a
86.92a

0.13
1.48
1.04
2.40

Halloumi II
8.54b
29.69b
37.50b
75.73b

0.22
1.24
1.60
2.44

Values are means standard errors.

Means within each row with a different superscript (a, b) differ signicantly (P 0.05).
Halloumi I: Halloumi cheese made by the cheese curd cooked for 30 min.
Halloumi II: Halloumi cheese made by the cheese curd cooked for 60 min.

None of the authors has a nancial or personal relationship with other people or organizations that could
inappropriately inuence or be perceived to inuence this
work.
Acknowledgements
Authors would like to thank very much Prof. Nikos
Moustakas and his laboratory for their aid with the atomic
absorption spectrophotometer.

114

S. Kaminarides et al. / Small Ruminant Research 125 (2015) 106114

Authors are grateful to Ms. Stavroula Perperidis and Mrs.

Elisabeth Wickham for their assistance and assiduity in
editing the study in the English language.
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