ORIGINAL PAPER

Physico-chemical, Sensory and Aromatic Properties of Cold PressProduced Safflower Oil

Buket Aydeniz • Onur Guneser • Emin Yılmaz

Received: 19 July 2013 / Revised: 13 September 2013 / Accepted: 16 September 2013 / Published online: 2 October 2013

� AOCS 2013

Abstract In this study, seeds from the safflower variety

called ‘‘Dincer’’ were roasted and microwaved before oil

extraction by cold pressing. Some physico-chemical anal-

yses (moisture, ash, oil content and color) were performed

in safflower meals. Physico-chemical properties (refractive

index, viscosity, turbidity, specific gravity, color, free

acidity, peroxide value, iodine number), nutritional com-

ponents (total phenolics, antioxidant capacity, tocopherol

content), sterol composition and fatty acid composition of

produced oils were also determined. Volatile components

of the oils were detected by solid-phase microextraction/

gas chromatography–mass spectrometry technique. Quan-

titative descriptive analysis was accomplished with trained

panelists by 11 definition terms. Cold pressing yielded less

oil than solvent extraction, but oil quality was superior and

a refining process was not required. There was no signifi-

cant difference between samples for fatty acid composition

and some physico-chemical parameters. Whereas, micro-

wave treatment caused a decrease in oil turbidity, free

acidity, a-tocopherol and some sterol contents and an

enhancement in total phenolic content, antioxidant capacity

and peroxide value. Moreover, microwave treatment led to

an increased nutty aroma in the oil. In contrast, isot pepper

aroma was decreased by microwave treatment. This study

provides very important information about the safflower

oils for the first time in the literature.

Keywords Safflower seed � Cold press � Oil quality �Volatile � Sensory � Tocopherol � Sterol

Introduction

Safflower (Carthamus tinctorius L.) is an ancient agricul-

tural crop widely cultivated worldwide and also a member

of Compositae family which includes artichoke, chicory

and sunflower. The parts of the plant can be used for dif-

ferent purposes as its colorful petals to prepare food col-

orants, flavorings, dyes and in medicine; seeds for

production of vegetable oils and bird feed, and foliage for

cattle feeding. Today it is cultivated in more than 30

countries with India, Mexico and US being the leading

ones. Since it is a drought and salt tolerant plant, it is

preferred in poor and dry lands as a suitable alternative

crop. Whole safflower seeds include 38–48 % oil, 15–22 %

protein and 11–22 % fiber. The hull makes up 18–59 % of

the seed weight and 1,000-seed weight ranges from 14 to

105 g, indicating great variation among different varieties

[1, 2]. In many parts of the world, safflower oil is used as

cooking oil due to its higher linoleic acid content and

characteristic nutty flavor with a distinct pale yellow to

golden color. Safflower oil is composed of 6–8 % palmitic,

2–3 % stearic, 16–20 % oleic and 71–75 % linoleic acids,

and exhibits the highest linoleic acid content among all the

commercial oils. As the main characteristics of the oil,

specific gravity of 0.919–0.924, refractive index of

1.473–1.476, titer of 15–17 �C, flash point of 121–149 �C,

free acidity of 0.15–0.60 %, saponification value of

186–194 mg KOH/g oil, iodine value of 141–147 g/100 g

oil, unsaponifiable matter of 0.3–0.6 %, peroxide value of

0–1.0 mequiv O2/kg oil (fresh oil), moisture and volatile

matter content of 0.03–0.1 % have been reported [1, 3, 4].

Vegetable oils from oilseeds are extracted by different

types of press systems, solvent extractors or a combination of

both. Generally, oilseeds contain higher levels of oil are first

pre-pressed and then solvent extracted, or direct solvent

B. Aydeniz � O. Guneser � E. Yılmaz (&)

Department of Food Engineering, Faculty of Engineering,

Canakkale Onsekiz Mart University, Terzioglu Campus,

17020 Canakkale, Turkey

e-mail: eyilmaz@comu.edu.tr

123

J Am Oil Chem Soc (2014) 91:99–110

DOI 10.1007/s11746-013-2355-4

extraction can be applied to materials with a lower oil level.

Selection of extraction technology is largely dependant on

the manufacturing cost, availability, material properties, the

usage goals of the cake (meal), environmental concerns and

others [5, 6]. Mechanical pressing is a simple and safe

technique, although more oil remains in the meal than by

solvent extraction. Occasionally, a special version of pressing

called ‘cold pressing’ is used to unique type of oil production.

In this technique, heating is not applied to oilseeds during the

pressing, moreover oilseeds must be very clean, uniform and

have an appropriate moisture level to be processed by cold

pressing. The cold pressing technique can yield very pure,

safe, nutritionally rich and sensorially acceptable virgin oils

which do not require refining and can be consumed directly.

However, the oil yield is usually lower than hot pressing and

solvent extraction. In order to enhance the oil yield of cold

pressing systems, some pre-treatments to whole oilseeds are

applied before pressing, e.g., microwave treatment, steaming,

enzyme application and pre-roasting. It is also indicated that

special cold pressed oils are high demand products in world

markets not only for food usage but also medicinal, cosmetic

and other uses [5, 7]. Gibbins et al. [8] found that aqueous

enzymatic extraction of safflower caused an enhancement of

yield but did not change the normal properties of the oils. Lee

et al. [9] investigated the effect of roasting temperature on

safflower oil composition and stability. They reported that the

roasting process led to improvements in the tocopherol

content and oxidative stability. In another study [10],

microwave treatment of rapeseed before cold pressing was

shown to enhance the oil yield, phytosterol and tocopherol

contents and oxidative stability.

Since cold press oils are virgin products, their aromatic

profiles and sensory properties are essential components for

consumer acceptance besides knowledge of their composi-

tion and nutritional quality. To the best of our knowledge,

there is no information about the volatile composition of cold

pressed safflower oil. In two earlier studies [11, 12] volatiles

of not safflower oil but safflower seeds were quantified. The

volatiles were extracted by microwave distillation or by

solvents extraction and analyzed by GC/MS techniques.

The aim of the present study was to investigate the

effects of regular roasting and microwave roasting treat-

ments on the safflower seeds prior to cold pressing and to

determine changes in physico-chemical parameters, nutri-

ent compositions, volatiles and sensory properties.

Experimental Procedures

Materials

In this study, one of the registered safflower varieties of

Turkey, called Dincer, was used. The seeds were harvested

in the 2011 autumn season, and cleaned for foreign mate-

rials. All other chemicals and standards were analytical

grade and purchased either from Merck (Darmstadt, Ger-

many) or Sigma-Aldrich (St. Louis, ABD).

General Analyses of the Safflower Seeds

Moisture content (%) was measured by an OHAUS

MB45 moisture analyzer (Ohaus, Pine Brook, NJ, US) at

110 �C with 1 g of sample for a 30-min drying program.

Total ash of the seeds was measured by the AOCS Ba 5a-

49 technique [13]. Oil content of the seeds was deter-

mined by the Soxhlet technique according to AOAC

920.39 [14]. Seed color was measured by a Minolta

CR300 colorimeter (Osaka, Japan). Seed length and

width were determined by a digital caliper (CD-15CP,

Mitutoyo Ltd, Andover, UK). The weight of 1,000 seeds

was calculated by weighing 100 seeds at least several

times and multiplying.

Seed Preparation for Cold Pressing

At the beginning of the study, cleaned and dried safflower

seeds were portioned for three equal amounts for control,

roasting and microwave treatments. Each portion was then

divided into two equal amounts for twice cold press oil

production. Pre-experiments had indicated that optimum

seed moisture content for cold pressing is 12 %, and for all

subsequent operations, the seed moisture level was con-

stantly measured and adjusted by addition of water. Water

content of the seeds reached equilibrium in hermetic bottles

by adding a calculated amount of water and storing at room

temperature overnight. The amount of water was calculated

from the equation [W = [(A/B) 9 C] - C], where W indi-

cates amount of added water, A indicates the dry matter

content of seed (%), B indicates the desired dry matter

content (%) of seed and C indicates the amount of

seeds (g).

Seed roasting was carried out using an air oven

(Ecocell Drying Oven, MMM Medcenter, Germany) at

140 �C for 45 min. The seeds were put in metal plate of

2 cm height, and the plate was stirred in every 15 min

during roasting. At the end of roasting time, seeds were

left to cool to room temperature and the moisture level

was measured and set to 12 % by addition of an appro-

priate amount of water.

Microwave treatment of the safflower seeds was carried

out in a microwave oven (Beko MD 1505, BEKO Elec-

trical Appliances, China) at 360 W for 6 min. The seeds

were put in a cylindrical Pyrex vessel (700 mL) and mixed

up at 3-min intervals. Then, the cooling and moisturizing

treatments were conducted by the same operations as the

roasting processes were repeated.

100 J Am Oil Chem Soc (2014) 91:99–110

123

Cold Pressing of the Safflower Seeds

Cold pressing of safflower seeds was performed on a lab-

oratory scale (12 kg seed/h capacity, single head, 2 hp,

1.5 kW power) cold press machine (Kocmaksan ESM

3710, Izmir, Turkey). For the press operation conditions,

10 mm exit die, 40-rpm screw rotation speed and a max

40 �C exit temperature were selected as constant parame-

ters. When oil (liquid phase) and oily cake-meal (solid

phase) were collected and weighed after each cold press-

ing, the oil was immediately filtered through a 40-lm

screen to separate suspended materials. Then, the oil was

centrifuged in a refrigerated centrifuge (Sigma 2–16K,

Postfach, Germany) at 8,603g for 10 min at 10 �C. The

clear upper oil phase is put into amber colored and capped

tubes, flushed with nitrogen and kept in a dark and cool

place until analysis. Oily cake or the meal, exiting from the

press die as 10–20 cm rods were first broken down in a

Warring blender (7011S, Warring Laboratory, US) and

then put into zipped refrigerator bags, labeled and frozen at

-20 �C until the analyses.

Analyses of the Safflower Seed Oily Cakes

Moisture content (%) was measured with an OHAUS

MB45 moisture analyzer (1 g sample, 110 �C and 30 min).

Total ash (%) and fat content (%) of the cakes were

determined by the AOCS Ba 5a-49 and AOAC 920.39

methods [13, 14], respectively. Color of the cakes was

recorded as L, a*, b* using a Minolta CR300 colorimeter.

Physical Analyses of the Safflower Seed Oils

The refractive index of oil samples was measured by an

Abbe 5 (Bellingham and Stanley, UK) refractometer at

25 �C, viscosity by a Brookfield viscosimeter (model DV

II ? Pro with Rheocalc software, Brookfield Eng. Lab.,

Inc., MA, US) equipped with an LV-SC4-18 spindle with

30 rpm at 25 �C. Specific gravity and turbidity (25 �C) of

the oils were measured by AOCS method Cc 10c-95

(AOCS 1984) using a Hach 2100 AN Turbidimeter (US).

CIE (L*, a* and b*) color values of the oils were measured

by a Minolta Colorimeter CR-200 (Minolta Camera Co.,

Osaka, Japan).

Chemical Analyses of the Safflower Seed Oils

Free fatty acid, peroxide and iodine number values of the

oil samples were determined according to AOCS methods

Ca 5a-40, Cd 8-53 and Cd 1-25 [13], respectively. Total

phenolics in the oil samples were first extracted with

water:methanol (60:40 v/v) at 1:1 ratio and then centri-

fuged at 6,797g at 4 �C for 10 min. The methanolic phase

was separated and the residue was re-extracted with the

same procedure. Finally, the extract was filtered through a

0.22-lm membrane filter. The same extracts were used for

both total phenolic content and antioxidant capacity

measurements.

Total phenolics of the oils were measured by the Folin-

Ciocalteu technique [15] with an Agilent 8453 UV–Vis

Spectrophotometer (Waldbronn, Germany) and calculated

as lg gallic acid equivalents per 100 g oil. The antioxidant

capacities of the oils were evaluated in the same extracts

[16] and expressed by the Trolox equivalent antioxidant

capacity defined as the lmol Trolox equivalents per g oil

sample.

Component Analyses of the Safflower Seeds Oils

The fatty acid compositions of the oil samples were

determined. The methyl esters of fatty acids were prepared

by AOCS method Ce 2-66 [17]. The quantification of fatty

acid methyl esters were analyzed with a gas chromatograph

(Finnigan Trace Ultra, Milan, Italy) equipped with an HP

88 capillary column (100 m 9 0.25 mm ID with 0.2 lm

film thickness; Agilent Technologies, Inc., Wilmington,

DE, US) and a mass spectrometer (Finnigan Trace DSQ,

Austin, TX, US) at 200 �C direct capillary interface tem-

perature, 70 eV ionization energy level, 50–500 amu mass

range with a 500-amu/s scanning rate. FAME mixture (37-

components, C4-C24, Supelco, Bellefonte, PA, US) and

CLA standards (Nu-Check, Elysian, MN, US) were used

for the determination.

Sterol composition of the oil samples was obtained by

the ISO 12228 method [18]. The samples were prepared

and injected with an autosampler into a Perkin Elmer

AutoSystem XL Gas Chromatograph equipped with an

FID, and a HP-5 (30m 9 0.32mm 9 0.25 lm) column.

The carrier gas was hydrogen with a 30-cm/s flow rate and

a 1:50–1:100 injector split ratio. The sample injection

volume was 0.2 lL and injector and the detector temper-

atures were 280 and 300 �C, respectively. The oven tem-

perature programme: initial temperature of 240 �C for

0.5 min, increased at 5 �C/min to 255 �C and was held for

4 min, then increased at 5 �C/min to 310 �C and held for

30 min. Instrumental control and data acquisition were

with Total Chrom Navigator version 6.3.1. Phytosterols

were determined by comparative retention times (relative

to 5a-cholestane) with those of commercially available

standards.

Tocopherol composition of the oil samples was analyzed

[19] using an Agilent HPLC series 1200 (Agilent, Wald-

bronn, Germany) with ChemStation software. The separa-

tion was with a ACE 5 SIL normal phase column (150 mm,

4.6 mm i.d., particle size 5 lm), and quantification was

with tocopherol standards (Merck, Darmstadt, Germany).

J Am Oil Chem Soc (2014) 91:99–110 101

123

Sensory Analysis of the Safflower Seed Oils

Sensory quantitative descriptive analysis (QDA) was used

to define cold pressed safflower oil samples [20–22]. A

panel composed of five females and four males aged

28–42 years took part voluntarily in the QDA of the oil

samples. Panelist training was completed for 10 h with

three seperate sittings in different days. During these panel

sessions, under the moderation of panel leader, the panel-

ists developed the sensory descriptive terms by using dif-

ferent fresh and refined safflower oil samples collected

from marketplaces. The standards used to calibrate the

panelists with the developed 11 descriptive terms are

shown in Table 1.

QDA was carried out by using a 10-cm scale anchored

from left zero to max intensity at right end. Within each

panel, three oil samples were coded with three-digit num-

bers and put into a colorless round-bottom and thinner head

glass closed with a metal lid. The safflower seed oil sam-

ples were served to the panelists at room temperature under

daylight with a serving of water, a slice of apple and an

expectoration cup. Duplicate samples were served in dif-

ferent sessions in a randomized order for each of the two

production samples.

Analysis of the Safflower Seed Oil Volatile Compounds

The volatile compounds in the safflower seed oils were

analyzed according to the technique of Krist et al. [23] with

minor modifications. Volatile compounds extraction was

completed with the solid-phase microextraction (SPME)

technique [24]. First, a 5-mL oil sample was weighed into a

40-mL amber SPME vial (Supelco, Bellefonte, US) and 1 g

NaCl and 10 lL of an internal standard were added. The

closed vial was vortexed for 1 min. Then, vial was put in a

water bath (GFL, Germany) at a constant 40 �C for 20 min

to equilibrate the volatiles in the headspace. Then, an

SPME (2 cm to 50/30 lm DVB/Carboxen/PDMS, Supe-

lco, Bellafonte) needle was inserted into the vial. The

SPME fiber was exposed at a depth of 2 cm in the head-

space of the vial for 20 min at 40 �C in a waterbath.

Finally, the fiber-collected volatiles was injected into a GC/

MS (Agilent 6890 N/Agilent 5875C mass spectrometer,

Agilent technologies, Wilmington, DE, US), immediately.

A nonpolar HP5 MS column (30 m 9 0.25 mm i.d. 9 0.25

lm film thickness, J&W Scientific, Folsom, CA) was used

for separation of the volatile compounds. The GC oven

temperature was programmed at 38 �C for 1 min., and

raised from 40 to 220 �C at 5 �C/min. The final oven

temperature held for 20 min. Helium was the carrier gas at

1.2 mL/min flow rate. The MSD conditions: capillary

direct interface temperature, 280 �C; ionization energy,

70 eV; mass range 35–350 amu; scan rate, 4.45 scans/s.

Identification of the volatiles was based on the comparison

of the mass spectra of unknown compounds with those in

the National Institute of Standards and Technology [25]

and Wiley Registry of Mass Spectral Data, databases [26]

and the Retention (Kovats) index. Volatile compounds

quantification were based on the relative abundances cal-

culated positively by the equation given below [24].

Methyl pentanoic acid and 2-methyl-3-heptanone were

used as internal standards (IS) for acidic and neutral-basic

characters compounds, respectively.

Mean relative abundance (lg/kg) = concentration of

IS 9 peak area of compound/peak area of the IS.

Statistical Analysis

The whole study was duplicated with all analyses within

each duplicate performed twice. Comparison of the control

and treatment groups for oil and oily cakes for the mea-

sured properties was accomplished by one-way ANOVA

and Tukey’s tests. Sensory analysis data was compared

with non-parametric Kruskal–Wallis and Dunn’s test. Sta-

tistical analyses were completed by using Minitab ver.

16.1.1 [27] and SPSS package [28] programs. For all sta-

tistical analyses, the level of confidence was at least 95 %

in this study.

Results and Discussion

According to Cosge and Kıralan [29], there are three cul-

tivars of safflower belonging to Turkey, namely Yenice,

Dincer and Remzibey-05. While Yenice and Dincer are

high linoleic acid cultivars, Remzibey-05 has a high oleic

acid content. The common properties of the safflower

cultivar ‘Dincer’ used in this study are shown in Table 2.

Table 1 Descriptive terms with references for the QDA of the saf-

flower seed oils

Descriptive term Reference standard

Isot pepper Wet isot pepper

Sunflower Sunflower seed

Nutty Roasted hazelnut

Hay Dry hay

Astringent Alum solution (0.1 %)

Waxy Melted paraffin

Spicy Chili pepper ? thyme in water

Earthy Humid soil

Bitter Caffeine solution (0.05 %)

Metallic A clean copper penny

Throat catching Harsh taste after 30 s when swallowed

102 J Am Oil Chem Soc (2014) 91:99–110

123

As seen in Table 2, the moisture, ash and oil contents

were 8.85, 1.76 and 27.76 %, respectively. The results are

in agreement with those in the literature. It was indicated

that the seed color depends on the variety; moreover the

seed color of Dincer was reported first time in this study.

The 1,000-seed weights and seed dimensions are also in

good agreement with those of the literature [1, 2, 30].

The general properties of the remaining oily cake after

the aforementioned pressing conditions are also shown in

Table 2. No significant differences (except b* value) were

observed in safflower meals samples (P [ 0.05). However,

microwaved treatment caused a higher b* value in saf-

flower meal than that of other treatments. Compared to

whole seed color (Table 2), the brightness of meals were

lower after crushing, evidenced by the reduction in the

L values.

The seeds in all treatment groups were set at a 12 %

moisture level before the press. Obviously, most of the

moisture was retained in the meals. Approximately

9.0–10.5 % of oil also remained in the cake after the

pressing. This is an unavoidable problem with the labora-

tory scale cold press machine used in our study. Depending

on the seed composition and structure, some part of the oil

could always remain in the cake or meal. This should be

taken into account when comparing the industrial press and

cold press for the oil yield and meal composition values. In

industrial type expeller presses, safflower meal contains

6.6 % crude fat, 21.03 % crude protein, 32.2 % crude fiber,

9.0 % moisture and 3.7 % ash. While pre-press-solvent

extraction had reduced the crude oil level to 0.5–1.5 %, but

not changed other components significantly [1].

Some important physico-chemical properties, total

phenolic and antioxidant capacity measures of the cold

press produced safflower oils are shown in Table 3. No

significant differences were observed in safflower samples

in terms of oil yield, refractive index, viscosity, a*, b*

color values and iodine value (P [ 0.05). However, in

practice oil recovery was a little higher in the roasted

samples (17.29 %) than those of control and microwaved

samples (16.71 and 16.18 %), respectively.

Since whole seed contained 27.76 % oil (Table 2)

determined by Soxhlet extraction, it can easily be said that

cold press is not as good as solvent extraction for oil gain.

On the other hand, cold press-produced virgin seed oils do

not need costly refining procedures. Only a filtration or

centrifugation is enough to get edible quality oils. In

addition, minor nutrients mostly lost during chemical

refining are retained in cold press oils. Depending on the

goal of production, end uses of both oil and meal, the

amount of seed that must be processed, a producer can

prefer a production type. Without question, full expeller

pressing and/or solvent extraction are the major oil pro-

duction techniques worldwide. Only for unique uses and

demands, are cold pressed seed oils produced [5, 6]. In one

study [8], aqueous enzyme assisted extraction of safflower

seed had the maximum oil amount and yield as 33.3 and

79.7 %, respectively. Clearly, the oil recovery rate was

higher than cold pressing. The refractive index, specific

gravity, free fatty acid value and iodine number of the

samples (Table 3) are in agreement with literature values

[1, 8]. The Codex Standard for named vegetable oils of

Turkey [31] permits up to 15 mequiv active oxygen/kg oil

for cold pressed and virgin oils. Obviously, microwave

treatment of the seeds caused the peroxide value to increase

significantly, compared to the control, but it is still below

the value of the codex limit. Turbidity of the microwaved

samples was significantly lower than others, and it can be

considered a good condition for filtration or centrifugation

costs to be reduced. In another study [10], rape seeds were

microwaved and their oxidative stability was measured by

Rancimat and found significantly higher than control oils.

Although they did not measure the peroxide value,

Table 2 General properties of the Dincer safflower seed and meals produced by cold pressing (mean ± SE)

Property Seed Property Meals

Control Roasted Microwaved

Moisture (%) 8.85 ± 1.28 Moisture (%) (P = 0.059) 11.73 ± 0.27 11.71 ± 0.30 12.60 ± 0.17

Ash (%) 1.76 ± 0.06 Ash (%) (P = 0.697) 2.44 ± 0.17 2.61 ± 0.16 2.54 ± 0.07

Oil (%) 27.76 ± 3.59 Oil (%) (P = 0.603) 9.12 ± 1.24 9.10 ± 1.54 10.64 ± 0.04

Color L 63.14 ± 0.25 Color L (P = 0.483) 47.86 ± 0.19 46.99 ± 0.52 47.65 ± 0.68

a* 1.90 ± 0.26 a* (P = 0.152) 2.08 ± 0.11 2.06 ± 0.07 2.56 ± 0.28

b* 15.96 ± 0.34 b* (P = 0.042) 11.16 ± 0.05AB 10.86 ± 0.37B 12.80 ± 0.75A

Seed length (mm) 7.71 ± 0.15

Seed width (mm) 4.68 ± 0.10

1,000-seed weight (g) 49.55 ± 1.54

SE Standard errorA,B Means followed by different superscript letters represent significant differences in the treatments for measured properties (P B 0.05)

J Am Oil Chem Soc (2014) 91:99–110 103

123

microwaved samples contained higher amounts of toc-

opherols and sterols. Table 3 also include viscosity, oil

color, oil total phenolics, and antioxidant capacity values of

the samples. Unfortunately safflower oil literature is absent

for those measurements in order to compare the values.

This study reports them first time for inclusion in the lit-

erature as very important data for cold pressed safflower

oil. Total phenolic content and antioxidant capacity values

of microwaved samples were significantly higher than

others indicating more minor component extraction after

microwave treatment, similar to the findings of a rapeseed

oil study [10].

The fatty acid composition of safflower oil samples in

this study are shown in Table 4. There were no significant

differences among the treatments in terms of the fatty acids

composition.

In fact, the measured fatty acid composition of the

samples are in very good agreement with those reported in

the codex [31] and other literature [1, 8, 9, 32]. It can be

claimed that neither roasting nor microwaving change fatty

acid composition of the cold press safflower oil. Similarly,

tocopherol composition of the oil samples is shown in

Table 4. Only a-tocopherol was quantified in the oil sam-

ples with the highest in roasted (502.12 mg/kg) and lowest

in the microwaved (366.24 mg/kg) samples. Lee et al. [9]

evaluated the effects of different roasting temperatures on

safflower oil components. They found 386–520, 8.9–12.4,

and 2.4–7.7 mg/kg oil of a-, b-, and c-tocopherols in saf-

flower oils, respectively. In addition, 5.8–7.0 and

7.5–8.4 mg/kg oil c- and d-tocotrienol were quantified.

Similarly, in the codex standard [31], the amounts of a-, b-,

and c-tocopherols and c-tocotrienol for crude safflower oil

were 234–660, 0–17, 0–12 and 0–12 mg/kg oil, respec-

tively. Franke et al. [33] reported 65.9, 1.8 and 0.7 mg/

100 g oil of a-, b- and c-tocopherols in safflower oil.

Although the amount of a-tocopherol measured in this

study is in good agreement with the previous studies, other

tocopherols and tocotrienols were not quantified. In addi-

tion, similar to the finding of Anjum et al. [34] for sun-

flower seed oils, microwave treatment caused a significant

decrease in the tocopherol level of the oil. The sterol

composition of the samples is also shown in Table 4. In

general, the concentrations of some phytosterols (campes-

terol, stigmasterol, D-5-23-stigmastadienol, b-sitosterol

and D-7-stigmastenol) were decreased significantly after

roasting or microwaving.

A contradictory result is reported for rapeseed oils, in

which after microwaving the phytosterol content were

enhanced by 15 % [10]. The phytosterol content of solvent

extracted safflower oil was reported [35]. The measured

values were of 290, 190, 1,450, 640, 710, and 190 mg/kg

fat of campesterol, stigmasterol, sitosterol, avenasterol, D-

7-stigmasterol and campestanol, respectively. Generally,

these values are higher than those measured in the present

study. It should be kept in mind that oil samples in this

study are cold-press produced, and clearly solvent extrac-

tion may yield more sterols in extracted oils.

The aromatic volatiles composition of the safflower oil

samples are shown in Table 5. Seventy-seven different

volatile compounds were quantified in the safflower oil

samples.

The volatiles quantified in all (control, microwaved and

roasted) samples are 2,3-butanediol, hexanal, ethylbenzene,

p-xylene, heptanal, a-pinene, p-cymene, D-limonene,

Table 3 Some physico-chemical properties, antioxidant capacity and total phenolics content values of the cold press extracted safflower seed

oils (mean ± SE)

Property Control Roasted Microwaved

Oil yield (%) (P = 0.732) 16.71 ± 0.61 17.29 ± 0.86 16.18 ± 1.25

Refractive index (25 �C) (P = 0.929) 1.47 ± 0.01 1.47 ± 0.01 1.47 ± 0.01

Viscosity (25 �C, cP) (P = 0.068) 42.97 ± 0.30 43.20 ± 0.45 44.20 ± 0.21

Turbidity (25 �C, NTU) (P = 0.013) 25.75 ± 4.25A 25.00 ± 6.65A 4.00 ± 0.57B

Specific gravity (20 �C) (P = 0.000) 0.92 ± 0.01A 0.92 ± 0.01A 0.92 ± 0.01A

Color L (P = 0.032) 34.05 ± 2.00B 35.90 ± 0.60AB 39.60 ± 0.49A

a* (P = 0.152) 1.33 ± 0.42 0.76 ± 0.12 0.54 ± 0.13

b* (P = 0.092) 30.08 ± 5.56 32.95 ± 2.93 42.47 ± 0.83

Free fatty acid (% oleic acid) (P = 0.011) 0.47 ± 0.022A 0.44 ± 0.03A 0.35 ± 0.01B

Peroxide value (mequiv O2/kg oil) (P = 0.01) 3.81 ± 0.87B 3.85 ± 0.76B 9.40 ± 1.58 A

Iodine number (g/100 g) (P = 0.202) 146.55 ± 4.71 143.29 ± 1.23 138.44 ± 1.51

Total phenolics (lg GA/100 g) (P = 0.001) 2616.10 ± 199.20B 2855.70 ± 217.80B 4079.30 ± 546.50A

TEAC (lmol Trolox/g oil) (P = 0.011) 309.33 ± 29.05B 315.32 ± 13.61B 538.26 ± 50.96A

SE standard errorA,B Means followed by different superscript letters represent significant differences in the treatments for measured properties (P B 0.05)

104 J Am Oil Chem Soc (2014) 91:99–110

123

1,5-octadien-3-ol, 2-octenal, nonanal, phenylethyl alcohol,

2-nonenal, 2,4-nonadienal, octanoic acid, naphthalene,

E,E-2,4-nonadienal, 3-dodecen-1-al, 2,4-decadienal, unde-

canal, E,E-2,4-decadienal, 2-dodecenal, 2-cyclohexen-1-

one, 5-tetradecene, 1-tetradecene, 2(3H)-furanone-dihydro-

5,5-dimethyl4-3-oxo-butyl, methyl eugenol, trans-caryo-

phyllene, tetradecenal, 2,4-dodecadienal, benzene-nonyl,

17-octadecenal, c-dodecalactone and 9-octadecanoic acid

methyl ester. Volatiles present only in microwaved samples

but not in the control and roasted samples are 2-methyl

butanol, pentanal, pyrazine, methyl pyrazine, furfural,

heptanone, pyrazine-2,5-dimethyl, hexanoic acid methyl

ester, 2-ethyl-pyrazine, 1-ethyl-2-formyl-pyrrol, 3,5-dime-

thyl-2-ethylpyrazine, 1-propyl pentyl ester butyric acid,

2-acetyl-6-methylpyrazine, E-3-nonene-2-one, 2-methyl-

5H-6,7-dihydrocyclopentapyrazine and tridecanoic acid.

Similarly, volatiles found only in the roasted samples can

be listed as; isoamyl alcohol, 1-phellandrene, isophytol and

2-N-heptyl furan. These results show that safflower oil is a

aromatics rich oil. Aromatic components associated with

oily, butter, creamy, fruity, green, plant, waxy, wood, cit-

rus, sweet, herbal, earthy, hay, pungent, bitter, spicy and

pepper sensory definitions are determined in almost all

samples. Microwave treatment was more effective than

roasting in the production of the pyrazine, furfural and

similar volatiles which are mostly responsible for the

roasted, nutty, caramel and similar aroma/flavor descrip-

tions. Aromatics with fruity, herbal and floral definitions

were present in roasted samples in addition to common

descriptors (Table 5). Unfortunately there is no study in the

literature about the volatile composition of safflower oils to

compare with this study. However, in two of the studies

Table 4 The fatty acid (%), sterol (mg/kg) and tocopherol (mg/kg) composition of the cold press extracted safflower oils (mean ± SD)

Fatty acids Control Roasted Microwaved

C12:0 0.26 ± 0.01 nd nd

C14:0 (P = 0.900) 0.25 ± 0.03 0.15 ± 0.02 0.15 ± 0.02

C16:0 (P = 0.956) 6.76 ± 0.62 6.79 ± 0.72 6.63 ± 0.04

C18:0 (P = 0.514) 2.50 ± 0.38 2.29 ± 0.09 2.21 ± 0.02

C18:1 (P = 0.523) 12.31 ± 2.25 12.29 ± 2.30 14.35 ± 0.03

C18:2 (P = 0.820) 76.92 ± 4.13 77.43 ± 3.34 75.50 ± 0.02

C18:3 nd nd nd

C20:0 (P = 0.550) 0.35 ± 0.02 0.35 ± 0.03 0.38 ± 0.01

C20:1 nd 0.16 ± 0.01 0.17 ± 0.01

C22:0 (P = 0.650) 0.25 ± 0.02 0.25 ± 0.03 0.27 ± 0.07

C22:6 (P = 0.286) 0.26 ± 0.03 0.27 ± 0.02 0.22 ± 0.02

Sterols Control Roasted Microwaved

Cholesterol nd nd nd

Brassicasterol nd 1.56 ± 0.01 nd

Ergosterol nd nd nd

24-Methylene cholesterol nd nd nd

Campesterol (P = 0.020) 274.0 ± 48.3A 124.53 ± 0.63B 120.08 ± 11.85B

Campestanol nd 10.31 ± 0.17 nd

Stigmasterol (P = 0.011) 133.1 ± 20.0A 54.95 ± 0.63B 56.50 ± 4.09B

D-7 Campesterol nd nd nd

D-5,23 Stigmastadienol (P = 0.046) 137.4 ± 41.6A 10.88 ± 0.11B nd

Cholesterol nd nd nd

b-Sitosterol (P = 0.028) 942 ± 177A 425.20 ± 2.43B 458.8 ± 48.5B

Sitostanol (P = 0.095) 45.40 ± 0.07 48.46 ± 0.96 54.60 ± 4.70

D-5 Avenasterol 32.8 ± 0.1 nd nd

D-5,24 Stigmastadienol nd nd nd

D-7 Stigmastenol (P = 0.014) 448.6 ± 68.5A 36.52 ± 0.15 B nd

D-7 Avenasterol 74.37 ± 7.54 nd nd

Tocopherol Control Roasted Microwaved

a-Tocopherol 2030.9 ± 16.6 1943.9 ± 66.6 1684.9 ± 13.8

nd not detected

J Am Oil Chem Soc (2014) 91:99–110 105

123

Table 5 Volatile compound composition of the cold press extracted safflower seed oil samples

Number RIa Name of the volatile Aroma/flavor description Concentration of the volatile compound (lg/kg oil)b

Control Microwaved Roasted

1 658 2-Methyl butanol Roasted, wine, onion, fruity nd 396.04 ± 10.55 nd

2 699 Pentanal Fermented, bread like,

fruity, nutty

nd 408.55 ± 222.43 nd

3 710 Acetoin Buttery, cheesy, milky,

sweet creamy, oily

1,256.39 ± 132.69 1,382.99 ± 115.01 nd

4 738 Pyrazine Pungent, sweet, corn like,

roasted, hazelnut

nd 178.41 ± 0.01 nd

5 742 Isoamyl alcohol Alcoholic, whiskey,

fruity banana

nd nd 720.90 ± 498.05

6 770 Methyl benzene (toluene) Sweet 884.73 ± 0.01 nd 1,134.66 ± 879.01

7 773 1-Pentanal Fermented, bread like,

fruity, nutty berry

338.87 ± 0.01 383.95 ± 8.14 nd

8 794 2,3-Butanediol Fruity, creamy-oily, butter 219.21 ± 0.01 218.88 ± 29.48 113.80 ± 21.97

9 800 Hexanal Green, fatty, leafy,

vegetable fruity

1,898.58 ± 497.61 2,336.27 ± 67.06 2,151.08 ± 699.58

10 825 Methyl pyrazine Nutty, brown, nut skin,

musty

nd 1,699.85 ± 343.77 nd

11 836 Furfural Sweet, woody, almond,

fragrant baked bread

nd 1,741.95 ± 356.30 nd

12 857 2-Hexenal Green, leafy, apple, plum 188.95 ± 0.87 nd 202.44 ± 90.36

13 864 Ethylbenzene Sweet, aromatic 147.91 ± 7.58 202.26 ± 62.04 213.99 ± 82.01

14 872 p-Xylene Fatty, cold meat 581.09 ± 12.08 1,193.29 ± 227.74 1,699.54 ± 0.01

15 891 Heptanone Fatty, fruity, spicy, sweet,

herbal coconut

nd 493.98 ± 98.80 nd

16 900 Heptanal Green, oily, plant, rancid,

waxy

564.56 ± 12.76 407.21 ± 128.67 345.04 ± 152.12

17 910 Pyrazine-2,5-dimethyl Cocoa, roasted nuts, roast

beef woody, grass

nd 1,208.66 ± 223.80 nd

18 913 c-Butyrolactone Creamy, oily, fatty, caramel 152.04 ± 14.02 nd 137.72 ± 37.79

19 926 Hexanoic acid, methyl ester Sweaty, sour nd 1,107.77 ± 0.01 nd

20 930 2-Ethyl-pyrazine Nutty, musty, fermented,

coffee roasted

nd 90.93 ± 27.07 nd

21 936 a-Pinene Woody-pine, terpentine,

spicy

58.43 ± 0.01 72.98 ± 1.58 41.19 ± 29.67

22 1,002 1-Phellandrene Citrus, herbal, terpene,

green peppery

nd nd 539.56 ± 12.79

23 1,025 p-Cymene Fresh, citrus, terpene,

woody spice

222.40 ± 0.01 229.62 ± 11.96 120.56 ± 71.61

24 1,030 D-Limonene Citrus, sweet, terpenic 57.81 ± 1.81 155.03 ± 6.44 179.22 ± 143.81

25 1,038 Benzyl alcohol Floral, phenolic, balsamic 158.74 ± 2.56 nd nd

26 1,041 1,5-Octadien-3-ol Earthy, mushroom,

geranium

112.52 ± 24.84 214.91 ± 62.91 77.51 ± 25.21

27 1,046 Benzene acetaldehyde Flower, honey, rose leaf 64.37 ± 0.01 100.14 ± 16.82 nd

28 1,052 1-Ethyl-2-formyl-pyrrol Burnt, roasted, smoky nd 107.75 ± 35.46 nd

29 1,060 2-Octenal Fatty, green, herbal 735.40 ± 1.65 510.11 ± 211.59 342.76 ± 149.67

30 1,078 Heptadecanoic acid – 147.09 ± 0.01 nd nd

31 1,085 Thiazolidine – 69.63 ± 0.01 210.26 ± 77.75 nd

32 1,087 3,5-Dimethyl-2-ethylpyrazine Potato, roasted, nutty nd 250.09 ± 47.18 nd

33 1,090 1-Propyl pentyl ester butyric

acid

Sweet, fruity, pineapple nd 881.26 ± 504.97 nd

34 1,092 Isophytol Mild, floral, herbal, green nd nd 202.31 ± 0.01

106 J Am Oil Chem Soc (2014) 91:99–110

123

Table 5 continued

Number RIa Name of the volatile Aroma/flavor description Concentration of the volatile compound (lg/kg oil)b

Control Microwaved Roasted

35 1,093 2-Hepten-1-ol Green, fatty 156.78 ± 0.01 nd nd

36 1,103 Nonanal Fatty, earthy 473.34 ± 5.61 509.56 ± 152.20 375.38 ± 432.21

37 1,114 Phenylethyl alcohol Rose 154.38 ± 0.01 179.84 ± 42.81 265.15 ± 52.11

38 1118 2-Acetyl-6-methylpyrazine Earthy, nutty, musty,

corn like

nd 159.22 ± 64.59 nd

39 1,141 (E)-3-Nonene-2-one Fruity, berry nd 82.93 ± 24.78 nd

40 1,143 2-Nonenal Hay, cucumber 267.20 ± 12.85 313.25 ± 108.76 207.65 ± 293.66

41 1,145 2,4-Nonadienal Fatty, green, cucumber 81.05 ± 4.66 80.08 ± 12.53 175.10 ± 0.01

42 1,173 Octanoic acid Fatty, waxy, rancid 185.08 ± 57.37 467.66 ± 0.01 766.77 ± 0.01

43 1,179 Benzaldehyde-4-ethyl Bitter, sweet, almond 31.96 ± 0.01 nd nd

44 1,183 Naphthalene Pungent, dry, tarry 62.99 ± 0.01 73.95 ± 22.35 121.82 ± 0.01

45 1,195 2-Methyl-5H-6,7-

dihydrocyclopentapyrazine

Roasted, nut nd 102.13 ± 34.15 nd

46 1,205 Decanal Soap, orange peel, tallow 124.751 ± 3.37 138.20 ± 10.30 nd

47 1,214 E,E,-2,4-Nonadienal Fatty, nutty, violet, leaf 81.05 ± 4.66 80.08 ± 12.53 73.59 ± 6.22

48 1,260 c-Octalactone Tobacco, coumarin-like,

sweet

46.19 ± 1.32 36.63 ± 13.62 nd

49 1,263 3-Dodecen-1-al Bitter, orange, mandarine

coriander

336.45 ± 0.01 227.65 ± 61.11 189.88 ± 135.33

50 1,266 c-Nonalactone Tropical, fruit, milky nd 75.21 ± 22.43 278.65 ± 394.08

51 1,278 6-Dodecanone Fruity, citrus, orange 75.14 ± 6.67 nd 155.98 ± 139.31

52 1,291 Thymol Herbal, thyme, phenolic 28.40 ± 6.46 nd nd

53 1,293 2,4-Decadienal Fatty, waxy, white meat

chicken

184.76 ± 20.93 133.47 ± 41.63 251.38 ± 280.72

54 1,297 2-N-Heptyl furan Green, fatty, lactonic, oily nd nd 51.28 ± 0.05

55 1,306 Undecanal Intensely soapy,

aldehydic wax

59.73 ± 8.68 52.28 ± 16.69 198.69 ± 601.76

56 1,316 (E,E)2,4-Decadienal Soapy 484.56 ± 62.11 362.16 ± 148.95 89.77 ± 126.96

57 1,344 5-Pentyl2(5H)-furanone Minty, fruity 45.88 ± 6.23 43.13 ± 19.12 nd

58 1,364 2-Dodecenal Green citrus, fruity,

mandarin orange, herbal

250.80 ± 1.20 198.30 ± 38.21 247.21 ± 219.44

59 1,379 2-Cyclohexen-1-one Green, roasted, savory 43.19 ± 10.34 34.88 ± 12.57 75.97 ± 29.57

60 1,380 4-Heptenal Oxidized fat 48.88 ± 6.75 34.88 ± 12.57 nd

61 1,386 5-Tetradecene Waxy, citrus 12.84 ± 2.12 16.11 ± 5.41 31.15 ± 10.96

62 1,390 1-Tetradecene Citrus, waxy, green pepper 38.55 ± 14.17 44.53 ± 18.64 67.24 ± 16.19

63 1,393 2(3H)-Furanone-dihydro-5,5-

dimethyl-4-3-oxo-butyl

– 15.70 ± 4.03 12.38 ± 4.23 95.38 ± 134.90

64 1,404 Methyl eugenol Sweet, fresh, warm, spicy 53.03 ± 43.85 20.53 ± 10.16 109.47 ± 96.04

65 1,408 Dodecanal Soapy, waxy, aldehydic,

citrus green, floral

44.90 ± 1.36 40.23 ± 13.24 nd

66 1,420 2,4-Undecadienal Fatty, waxy, chicken nd 29.43 ± 8.57 51.69 ± 30.53

67 1,424 trans-caryophyllene Sweet, woody, spice 52.20 ± 32.72 55.93 ± 18.94 56.47 ± 23.77

68 1,454 cis-geranyl acetone Fresh green, fruity, waxy,

rose

49.83 ± 1.37 15.28 ± 5.58 nd

69 1,510 Tetradecanal Fatty, waxy, dairy, creamy 25.31 ± 4.41 20.83 ± 4.44 81.10 ± 15.55

70 1,524 2,4-Dodecadienal Grapefruit, orange, fatty,

citrus

6.36 ± 5.56 10.74 ± 2.81 31.15 ± 10.54

71 1,561 Lauric acid Metallic nd 23.36 ± 19.55 84.52 ± 64.92

72 1,570 Benzene-nonyl – 19.88 ± 2.74 13.26 ± 2.33 151.20 ± 29.37

J Am Oil Chem Soc (2014) 91:99–110 107

123

[11, 12] volatiles of not safflower oil but safflower seeds

were quantified. In one study, microwave distillation and

solid-phase microextraction coupled with gas chromatog-

raphy-mass spectrometry and 32 volatile compounds were

separated and identified from safflowers. The most abun-

dant compounds were paeonol, a-asarone, b-asarone,

1-methyl-4-(2-propenyl)-benzene and diethenyl-benzene

[11]. When compared to the volatiles presented in Table 5,

benzene acetaldehyde, naphthalene, 3-dodecen-1-al,

5-pentyl2(5H)-furanone, 2-cyclohexen-1-one, methyl

eugenol, dodecanal, caryophyllene, geranyl acetone, te-

tradecanal, tridecanoic acid and 17-octadecenal are the

similar compounds identified in both studies. Similarly,

volatile components of safflower were extracted by

solvents and analyzed by GC/MS, and 20 components were

identified in another study. Hexadecanoic acid, heneico-

sane, nonacosane, 7,9-docosanedione, octadecanoic acid,

(Z,Z,Z)-9,12,15-octadecatrienoic acid methyl ester, penta-

cosane and nonacosanol were found with the highest fre-

quency [12]. Only heptadecanoic acid, octanoic acid,

tetradecanal, dodecalactone were similar compounds in

both studies. But most importantly, it must be kept in mind

that volatiles in safflower seeds and oils extracted from

those seeds can be very different since the biomaterial

changes significantly. This study provides the first data for

the volatile compounds composition of safflower seed oils.

Descriptive sensory analysis (QDA) results of the saf-

flower seed oil samples in the spider web form are shown

in Fig. 1.

The panel described the samples with 11 sensory terms,

and except nutty term, there was no statistically significant

differences between the samples. The nutty score was

highest in the microwaved sample, where also the pyrazine

and furan compounds were in high concentrations

(Table 5). Isot pepper was a very distinct defining aroma for

these oils. Isot pepper also known as Urfa pepper (Capsicum

annuum L.) is a dried type of pepper having a typical

smoky, raisin-like taste and fermented aroma with deep

purple to a dark purplish black color. It is less spicy than

most chili peppers, but yields a more lasting heat on the

tongue [36]. The isot pepper aroma was lowest in micro-

waved (1.66), and highest in the control (2.36) samples.

This score was, in fact, the largest among all the sensory

definitions terms. Contrarily, the terms of sunflower and

nutty were highest in the microwaved samples (2.00 and

2.97, respectively) than control (1.86 and 1.72) and roasted

(1.83 and 1.52) samples. Hay, waxy, spicy and earthy scores

were higher than 1.00, but not different between the sam-

ples. There are also detectable levels of bitter, metallic and

throat-catching sensations measured in the samples.

Table 5 continued

Number RIa Name of the volatile Aroma/flavor description Concentration of the volatile compound (lg/kg oil)b

Control Microwaved Roasted

73 1,660 Tridecanoic acid (myristic acid) Waxy, woody nd 7.59 ± 0.01 nd

74 1,714 17-Octadecenal Fatty, waxy 20.46 ± 3.93 17.51 ± 0.97 134.44 ± 0.62

75 1,827 Isopropyl myristate Faint, oily, fatty 31.08 ± 22.80 28.36 ± 21.87 nd

76 2,109 c-Dodecalactone Fatty, peach, sweet,

metallic

28.51 ± 0.55 32.46 ± 0.01 176.17 ± 58.39

77 2,127 9-Octadecanoic acid, methyl

ester

Mild, fatty 97.05 ± 35.53 528.65 ± 582.76 213.12 ± 0.01

nd not detecteda RI (Kovats Index) on HP 5MS columnb Mean relative abundance = (concentration of internal standard 9 peak area of compound)/(peak area of the internal standard)

Fig. 1 Spider web representation of the QDA results of the safflower

seed oils

108 J Am Oil Chem Soc (2014) 91:99–110

123

Clearly, the treatment of microwaving has enhanced sen-

sory properties of the samples, evidenced by the reduction

of unwanted aromas and enhancement of the positive terms.

Volatile compounds with roasted, nutty, hazelnut, caramel,

fresh, green, spicy, pepper, herbal, hay, leaf and similar

definitions were identified in the samples (Table 5), are also

in good agreement with the sensory descriptions determined

by the panel (Fig. 1) for the same oils. Most importantly,

this study provides the first sensory descriptions of the

safflower oil samples.

Conclusion

Safflower seed oil can be produced by the cold pressing

technique giving edible quality which does not require

chemical refining, only a simple filtering or centrifugation to

remove suspended plant materials may be needed. Roasting

and microwave treatment before pressing did not change the

oil specifications significantly, but especially microwave

treatment caused oil turbidity, free acidity, a-tocopherol and

some sterol levels to be reduced; and the total phenolic

content, antioxidant capacity and peroxide value to be

enhanced significantly. In addition, the oil sensory descrip-

tors of isot pepper and nutty did show some changes caused

by the treatments. While the oil recovery rate was not sig-

nificantly different between the pre-treated and control

samples, some oil quality parameters and sensory descrip-

tors were better with oils produced from microwaved seeds.

Volatile compositions and sensory descriptions of safflower

seed oils were provided for first time with this study for a

valuable contribution to the literature.

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