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ARTICLE IN PRESS

JOURNAL OF
FOOD COMPOSITION
AND ANALYSIS
Journal of Food Composition and Analysis 20 (2007) 202–211
www.elsevier.com/locate/jfca

Original Article

Physicochemical and quality characteristics of cold-pressed flaxseed oils


Wee-Sim Choo, John Birch, Jean-Pierre Dufour
Department of Food Science, University of Otago, New Zealand, Dunedin 9015, New Zealand
Received 24 March 2006; received in revised form 1 December 2006; accepted 15 December 2006

Abstract

Flaxseed oils currently sold on the worldwide market are not governed by specific standards or specifications. In this study, the
physicochemical and quality characteristics of seven cold-pressed flaxseed oils sold in New Zealand have been analyzed. General
regulations and specification for edible vegetable oils and cold-pressed oils were used as a guide. Fatty acid composition, tocopherol
composition, moisture and volatile matter content, free fatty acids, chlorophyll pigments, total phenolic acids, total flavanoids, acid
value, unsaponifiable matter, peroxide value, conjugated dienoic acids, p-anisidine value and specific extinction in the ultraviolet
spectrum of the flaxseed oils were measured. Color and dielectric measurement of the flaxseed oils were also estimated using a
spectrocolorimeter and a food oil sensor, respectively. The physicochemical characteristics of the flaxseed oils were found to be quite
similar with only a few significant variations. Four out of the seven flaxseed oils passed all the quality tests conducted in this study.
r 2006 Elsevier Inc. All rights reserved.

Keywords: Flaxseed oil; Omega-3 fatty acid; Alpha-linolenic acid; Oil quality; Food safety; Food quality

1. Introduction dietary recommendations, Deckere et al. (1998) reported


that an intake of 2 g/day or 1% of energy of ALA appears
Flax (Linum usitatissimum) is an economically important prudent whereas Simopoulos et al. (2000) reported
oilseed crop (Oomah, 2001; Lei et al., 2003) containing 0.65 g/day of docosahexaenoic acid (DHA) plus eicosa-
about 40% oil in the seed. Flaxseed (also known as linseed) pentaenoic acid (EPA), and 2.22 g/day of ALA as the
is regaining its popularity from its traditional usage as a adequate intake (AI) for adults. The AI is a value based on
raw material in oil production because of the reported experimentally derived intake levels or approximations of
health benefits of n-3 fatty acids and its exceptionally high observed mean nutrient intakes by a group (or groups) of
content of the n-3 fatty acid, alpha linolenic acid (ALA). healthy people and this reference intake is used instead of
According to Daun et al. (2003), flaxseed oil usually recommended dietary allowance if sufficient scientific
contains greater than 50% of ALA. Supplements contain- evidence is not available to calculate an estimated average
ing flaxseed oil, mostly in gelatin capsules, are being sold in requirement (Simopoulos et al., 2000).
health food stores and marketed over the Internet. Cold- The high content of ALA in flaxseed oil is, however,
pressed flaxseed oil is also commercially available in low- highly susceptible to oxidation, leading to rapid deteriora-
and high-lignan forms in the North American market tion of quality. Lukaszewicz et al. (2004) reported that even
(Morris and Vaisey-Genser, 2003). Consuming flaxseed oil after cold extraction, to avoid rapid appearance of
is one good way to increase the n-3 fatty acids in the diet as rancidity, flaxseed oil is often supplemented with vitamin
most societies nowadays are known to generally consume E, stored in dark glass jars and may not be used for frying.
plenty of n-6 fatty acids in processed foods, margarine and There is one standard that applies to conventional linseed
vegetable oils and the absolute amounts of n-3 fatty acids oil, American Society for Testing and Materials (ASTM) D
in the diet are too low. With regard to n-3 fatty acids 234-82 (1998), which covers the properties of raw linseed oil
and the applicable test method (Kolodziejczyk and Fedec,
Corresponding author. Tel.: +64 3 4797566; fax: +64 3 4797567. 1995). The International Organization for Standardization
E-mail address: john.birch@stonebow.otago.ac.nz (J. Birch). (ISO) 5513-1982 ‘‘Linseed for the Manufacture of Oil’’

0889-1575/$ - see front matter r 2006 Elsevier Inc. All rights reserved.
doi:10.1016/j.jfca.2006.12.002
ARTICLE IN PRESS
W.-S. Choo et al. / Journal of Food Composition and Analysis 20 (2007) 202–211 203

Specification, which specifies flaxseed requirements for the in preparing the oils are to be free from pests, ergot,
manufacture of oil for industrial use including foodstuffs poisonous seeds, mycotoxins, mould, mites and any
was withdrawn on 18 November 1994. As there is no specific bacterial-related diseases, The minimum oil content of
standard or specification available for the use of flaxseed oil the seed is 36%. Desirable moisture content and acid value
in the food sector, standard qualities and compositions of of the seed are below 8% and 2%, respectively. All the
other unrefined, edible vegetable oils were used as a guide. chemicals and solvents used were of analytical or HPLC
Among the standards used were Codex Alimentarius grade.
Commission (1999) standard for virgin oils and cold-pressed
fats and oils, New Zealand Food Regulation (1984) 2.2. Methods
specification for edible and virgin fats and oils, and
Australia New Zealand Food Authority (2000) for edible 2.2.1. Fatty acid composition
oils. The objective of this research was to analyze the Fatty acid composition was determined using gas
physicochemical and quality characteristics of cold-pressed chromatography of fatty acid methyl esters (FAME).
flaxseed oils sold in New Zealand. Seven cold-pressed FAME were prepared according to the method of van-
flaxseed oils were available at the market at the time of Wijngaarden (1967) with some modifications. Approxi-
study and therefore were analyzed. mately, 20 mg of sample was weighed into a glass tube
(15.0 cm  1.3 cm with Teflon-lined screw cap) and 2 mL of
2. Materials and methods 0.5 N methanolic sodium hydroxide was added. The
mixture was boiled for 20 min and then cooled to room
2.1. Materials temperature. About 2 mL of diethyl ether and 5 mL of
water were added and mixed well by tilting the capped tube
Details of the seven cold-pressed flaxseed oils used are with no shaking of the tube. The ether layer was then
given in Table 1. Basic quality parameters of the seeds used discarded and the aqueous layer was acidified with

Table 1
The names of the flaxseed oils, together with their source, bottle volume, relative cost and remarks on their bottle labels

Flaxseed oil Abbreviated Source Bottle Cost/mL Organic Remarks on Storage instruction
name volume (cents)a certification label

Waihi Bush organic WB South 250 mL 5 Yes Not for cooking Once opened, keep
farm flaxseed oil Canterbury refrigerated. Once
opened use within 5
weeks. Can be frozen.
500 mL
Melrose organic MEL Bottled in 250 mL 8 Yes Do not heat Store under
flaxseed oil Australia from refrigeration. Use
imported within 8 weeks of
flaxseed oil opening. May be
frozen with confidence.
500 mL
b
Oil seed extractions OSELC Canterbury — None — If stored in unopened
limited flaxseed oil Plains containers at under 20
1C, this product can be
expected to have a
shelf life of 12 months.
b
Oil seed extractions OSELO Canterbury — Yes —
limited organic Plains
flaxseed Oil
Good health FO Canterbury 250 mL 6 Yes Not suitable for Keep refrigerated and
FlaxOmegaTM extra Plains heating use within 3 months of
virgin high lignan flax opening. Can be
oil frozen.
Essential body EBN Canterbury 250 mL 4 None Not suitable for Best kept refrigerated.
nutrition flaxseed oil Plains cooking
500 mL
Healtheries flaxseed oil HEA Packed in New 500 mL 4 None Not suitable for Store below 30 1C.
Zealand from heating
imported
flaxseed oil
a
Cost was calculated based on 500-mL price.
b
Oil seed extractions limited supply flaxseed oil in bulk.
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concentrated HCl. Acidity was checked using Litmus in a vacuum rotary evaporator at 40 1C. The residue was
paper. The aqueous layer was backwashed with a further dissolved in 1 mL methanol and stored at 20 1C prior to
2 mL of diethyl ether and then transferred to a new Kimax analysis. The spectrophotometric determination of flava-
tube. About 1 mL of BF3-methanol reagent (BDH noid content was carried out according to the method of
Laboratory Supplies, Poole, England) was added and the Oomah et al. (1996). About 1 mL of the methanolic extract
mixture was boiled for 20 min. About 5 mL of saturated was diluted 3  with distilled water and absorption was
sodium chloride solution was then added. About 1 mL of measured at 404 nm using an Ultraspec 3300 pro spectro-
the upper (diethyl ether) layer was pipetted into a 2-mL photometer (Amersham Pharmacia Biotech, Uppsala,
sample vial. This solution (FAME) was quantified on an Sweden) after the addition of 100 mL of 1% 2-amino-
Agilent 6890N gas chromatograph, equipped with an ethyl-diphenylborate (Sigma Chemical Co., St. Louis, MO,
Agilent 7683 series autosampler (Agilent Technologies USA) solution. Luteolin (Sigma Chemical Co., St. Louis,
Inc., Wilmington, DE, USA) and a flame ionization MO, USA) served as a standard for preparing the
detector. The FAME in diethyl ether (1 mL) was injected calibration curve ranging from 0 to 42 mg luteolin/3 mL
into the column with a split ratio of 40:1. The injector and assay solution in 80% methanol. The concentration of total
detector temperature were set at 250 1C. Hydrogen was phenolic acids was determined according to the method of
used as the carrier gas at a flow rate of 2 mL/min. Gutfinger (1981). The procedure consisted of dilution of
Separation was carried out on a BPX70 capillary column 0.1 mL of the methanolic extract with water to 5 mL in a
(50 m  330 mm, SGE International Pvt. Ltd., Victoria, 10-mL volumetric flask, and addition of 0.5 mL Folin-
Australia) with a film thickness of 0.25 mm. The column Ciocalteau’s phenol reagent (2 N; Sigma Chemical Co.,
temperature was programmed from 35 to 205 1C at St. Louis, MO, USA). After 3 min, 1 mL of saturated
2.5 1C/min and then to 230 1C at 10.0 1C/min and was held (ca. 35%) Na2CO3 solution was added. The contents were
at 230 1C for 20 min. The resultant data were processed by mixed and diluted to volume with water. The extinction
a computer using HP Chemstation software (Hewlett was measured after 1 h at 725 nm against a reagent blank.
Packard, Agilent Technologies Inc., Wilmington, DE, Ferulic acid (Sigma Chemical Co., St. Louis, MO, USA)
USA). Identification of fatty acids was carried out using served as a standard for preparing the calibration curve
a reference standard mixture FAME Q005 (Nu-Check ranging from 0 to 400 mg/mL assay solution.
Prep, Inc., Elysian, MN, USA) analyzed under the same
operating conditions as those employed for FAME of the
samples. 2.2.7. Tocopherol composition
Tocopherol composition of the flaxseed oils was
2.2.2. Moisture and volatile matter content determined using high performance liquid chromatography
Moisture and volatile matter content of flaxseed oils according to A.O.C.S. Recommended Practice Ce 8-89
were determined according to A.O.C.S. Recommended (1998). Samples (10 mL) were analyzed by an HPLC system
Practice Ca 2d-25 (AOCS, 1998). consisting of a Varian 9010 solvent delivery system (Varian
Associates, Inc., Walnut Creek, CA, USA) with an injector
2.2.3. Unsaponifiable matter of 10 mL loop size, an SPD-M10AV diode array detector
Unsaponifiable matter of the flaxseed oils was deter- (Shimadzu, Kyoto, Japan) set at 298 nm, and analyzing
mined according to A.O.C.S. Recommended Practice Ca software, Shimadzu Class-M10A. An analytical prepacked
6a-40 (AOCS, 1998). column (4.6  250 mm2), SphereClone 5 mm Silica (Phe-
nomenex, Torrance, CA, USA) was used with propan-2-ol
2.2.4. Free fatty acids in hexane (0.5:99.5, v/v) as the mobile phase. The system
Free fatty acids of flaxseed oils were determined was operated isocratically at a flow rate of 1 mL/min.
according to A.O.C.S. Recommended Practice Ca 5a-40 Typically, a 10-min equilibration period was used between
(AOCS, 1998). samples, requiring about 40 min/sample. Quantification
was based on an external standard method. Mixed
2.2.5. Chlorophyll pigments tocopherol standards in hexane solution (2 mg/mL), were
Chlorophyll pigments of flaxseed oils were determined prepared from standard compounds: a-, g-, d-tocopherol
according to A.O.C.S. Recommended Practice Cc 13i-96 (Sigma Chemical Co., St. Louis, MO, USA) and rac-b-
(AOCS, 1998). tocopherol (Supelco, Bellefonte, PA, USA). Qualitative
and quantitative determination of plastochromanol-8 was
2.2.6. Total phenolic acids and flavanoids carried out according to the method of Balz et al. (1992).
Extraction of phenolic acids and flavanoids was carried
out according to the method of Vazquez Roncero et al.
(1973, cited in Gutfinger, 1981). Ten grams of oil was 2.2.8. Color
dissolved in 50 mL hexane and the solution was extracted Color of the flaxseed oils was determined using CIELab
successively with three 20-mL portions of 60% aqueous color scales with a MiniScan XE spectrocolorimeter
methanol. The combined extracts were brought to dryness (Hunterlab, Reston, VA, USA).
ARTICLE IN PRESS
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2.2.9. Peroxide value 3. Results and discussion


Peroxide values of the flaxseed oils were determined
according to A.O.C.S. Recommended Practice Cd 8-53 Table 2 shows a summary of the fatty acid composition,
(AOCS, 1998). percent of unsaturated fatty acids and ratios of n-3 to n-6
fatty acids of the seven cold-pressed flaxseed oils. Fatty
2.2.10. Conjugated dienoic acids acid analysis of 11 cultivars of flaxseed grown in North
Spectrophotometric determination of conjugated dienoic Dakota, USA gave 45–52% ALA whereas the mean value
acid of the flaxseed oils was determined according to of ALA content of Western Canadian flaxseed based on
A.O.C.S. Recommended Practice Ti 1a-64 (AOCS, 1998). analysis of 495 samples was 59% (Bhatty, 1995). The ALA
content of New Zealand-grown flaxseed oils were quite
2.2.11. p-Anisidine value similar to that of oils from Canadian-grown flaxseed but
p-Anisidine values of the flaxseed oils were determined were higher than that of oils of US-grown flaxseed.
according to A.O.C.S. Recommended Practice Cd 18-90 OSELC, FO and EBN had the highest levels of ALA
(AOCS, 1998). (58.87–60.42%) and lowest levels of oleic acid
(13.44–14.65%). These results agree with Bhatty (1995)
who reported that with an increase in ALA in flaxseed oil,
2.2.12. Acid value
there was a corresponding decrease in oleic acid. HEA had
Acid values of flaxseed oils were determined according to
the lowest ALA and highest oleic contents at 51.80% and
A.O.C.S. Recommended Practice Cd 3d-63 (AOCS, 1998).
22.21%, respectively, and these amounts were significantly
different (po0.05) from the other oils. This may be due to
2.2.13. Specific extinction in ultraviolet spectrum a different flaxseed variety, origin and its corresponding
Specific extinction of flaxseed oils at the wavelengths of environmental variation.
230 and 270 nm were determined according to IUPAC Table 3 shows selected physicochemical characteristics of
method II.D.23 (IUPAC, 1979). the seven cold-pressed flaxseed oils. Waxes, sterols and
hydrocarbons in oils are generally determined as unsapo-
2.2.14. Dielectric measurement nifiable matter (Stauffer, 1996). Water contributes to the
Dielectric measurement of the flaxseed oils was carried hydrolysis of oil during various handling and processing
out with a food oil sensor (Northern Instruments steps, which generates free fatty acids and glycerol
Corporation, Lino Lakes, MN, USA). products. Thus, it is desirable to have low moisture content
in oils. According to the Australia New Zealand Food
2.3. Statistical analysis Authority (2000), edible oils may contain incidental
amounts of free fatty acids, unsaponifiable constituents
Data were interpreted by analysis of variance (ANOVA) and other lipids.
with Duncan’s multiple-range test using SAS software Lipid oxidation is the main process leading to the
package (SAS Institute Inc., Cary, NC, USA). The deterioration of edible oils, e.g. during production,
statistical significance was evaluated at po0.05 level. transportation and mainly storage (Hrncirik and Fritsche,

Table 2
Summary of fatty acid composition (% fatty acid), % unsaturated fatty acids and ratio of omega 3–6 fatty acids

Fatty acid WB MEL OSELC OSELO FO EBN HEA

C16:0 6.4770.06a 5.6770.07d 5.8170.24bc 5.9370.20b 5.7370.06cd 5.5270.14e 5.4870.09e


C16:1 0.0770.01cd 0.0970.01ab 0.0870.02cd 0.0970.02ab 0.0570.03d 0.0870.02ab 0.1070.01a
C17:0 0.0770.01ab 0.0770.00ab 0.0870.02ab 0.0770.02ab 0.0770.00ab 0.0670.00b 0.0670.00b
C18:0 2.8570.04c 3.8470.33a 3.2170.21b 4.0970.26a 2.2470.01d 3.3170.47b 3.9270.28a
C18:1 17.2270.16d 21.6670.14b 14.6570.13e 18.3270.08c 13.4470.09f 14.5470.21e 22.2170.89a
C18:2 15.4570.05d 15.3170.30de 15.9370.12b 15.1770.31e 17.4470.05a 15.6970.23c 15.7770.09bc
C18:3 57.2570.29b 54.1173.03c 59.6070.48a 56.4571.30b 60.4270.25a 58.8772.59a 51.8071.38d
C20:0 0.1570.01a 0.1670.04a 0.1670.01a 0.1770.03a 0.1370.01b 0.1570.02a 0.1670.01a
C20:1 0.1670.01b 0.1570.00c 0.1570.00c 0.1370.01e 0.1470.00d 0.1670.01bc 0.2070.02a
C20:2 0.0270.02bc 0.0470.02ab 0.0270.02bc 0.0170.02c 0.0270.02a 0.0670.02a 0.0570.04ab
C20:3 0.0670.00c 0.0570.01cd 0.0870.00ab 0.0670.01c 0.0970.00a 0.0770.03bc 0.0470.02d
C22:0 0.1470.00a 0.1470.01a 0.1370.01ab 0.1470.01a 0.1170.00b 0.1270.02ab 0.1370.02ab
C24:0 0.1070.01a 0.1070.01a 0.1070.01a 0.1070.01a 0.0870.01c 0.0870.02bc 0.0970.01ab

% Unsaturated fatty acids 90.2370.08cd 89.8470.11de 90.5070.49c 89.4670.06e 91.6170.11a 91.0070.31b 90.1470.42cd
Omega-3: omega 6 fatty acids 3.7070.03a 3.4770.02b 3.7470.03a 3.7270.01a 3.4770.02b 3.7270.14a 3.2870.10c

Values are means7standard deviations of five (n ¼ 5) measurements.


abcde
Values with different superscript letters within a row are significantly different at po0.05.
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Table 3
Physicochemical characteristics of flaxseed oils

WB MEL OSELC OSELO FO EBN HEA

Moisture and volatile 0.6570.03b 0.5170.04cd 1.0370.06a 0.7170.02b 0.4570.04d 0.5470.03c 1.0870.04a
matter content (%)
Unsaponifiable 0.3970.17b 0.7170.07a 0.5770.18ab 0.4470.14ab 0.4170.05ab 0.3970.12ab 0.5870.15ab
matter (%)
Free fatty acids, as 0.2570.04e 0.4270.03d 0.8170.05b 0.3070.07e 0.6070.08c 0.4470.05d 0.9870.06a
oleic (%)
Chlorophyll 1.2670.01e 1.3770.01d 0.8070.02g 1.9570.02c 5.7670.02a 0.8770.01f 3.7270.01b
pigments content, as
mg of pheophytin a/
kg of oil
Total flavanoid, as 15.170.8de 25.670.4a 22.272.7ab 12.771.8e 14.172.0de 19.873.2bc 16.971.8cd
luteolin equivalents
(mg/100 g)
Total phenolic acids, 121.7719.9cd 87.2715.0d 218.1732.3b 76.8711.2d 148.4725.0c 140.9713.4c 307.3741.5a
as ferulic acid
equivalents (mg/
100 g)

Values are means7standard deviations of three (n ¼ 3) measurements.


abcdef
Values with different superscript letters within a row are significantly different at po0.05.

2005). The oxidation of oils and particularly polyunsatu- group (Larson, 1997). Phenolic acids are natural hydrophilic
rated vegetable oil such as flaxseed oil may be accelerated antioxidants, which occur ubiquitously in fruits, vegetables,
by exposure to light. Photooxidation provides an impor- spices and aromatic herbs (Silva et al., 2000). The total
tant way to produce hydroperoxides from unsaturated phenolic acids content of flaxseed meal on a dry-weight
fatty acids and esters in the presence of oxygen, light basis, as reported by Wanasundara and Shahidi (1994)
energy and a photosensitizer. Chlorophyll pigments in oil ranges from about 130 to 220 mg/100 g, as ferulic acid
can initiate photosensitized oxidation (Frankel, 2005). FO, equivalents. Both MEL and OSELO were at the lower end
a high lignan cold-pressed flaxseed oil has the highest of total phenolic acids content (76.8–87.2 mg/100 g) whereas
chlorophyll pigment content among all oils. This may be HEA showed the highest total phenolic acids content at
due to the addition of 2% lignan particulates within the 307.3 mg/100 g of oil, being almost four times higher than
flaxseed back into the cold-pressed oil. According to MEL and OSELO.
Wiesenborn et al. (2003), lignan occurs mainly in the hull Table 4 shows the tocopherol and plastochromanol-8
of flaxseed. However, the chlorophyll pigment contents of content of the seven cold-pressed flaxseed oils. Tocopherols
the seven cold-pressed flaxseed oils were much higher than and plastochromanol-8 are natural lipophilic antioxidants
those in fully refined soybean and canola oils but lower found in vegetable oils. OSELO has the highest total
than that found in crude pressed canola oils as reported by tocopherol plus plastochromanol-8 content among all the
Usuki et al. (1984) and Endo et al. (1992). oils. Both HEA and MEL were at the lower end of the total
Flavanoids are a group of natural benzo-g-pyrane tocopherol plus plastochromanol-8 content. a-tocopherol
derivatives ubiquitous in the plant kingdom, and exert was found at relatively low concentrations in most of the
multiple biological effects including antioxidative activity cold-pressed flaxseed oils, which varied between 0.00 and
(Pekkarinen et al., 1999). Flavanoids have been reported by 0.55 mg/100 g of oil, except for OSELO which showed
Nieto et al. (1993) and Hudson and Lewis (1983) to have an exceptionally high concentration of a-tocopherol
the potential to function as antioxidants in food lipid (9.11 mg/100 g of oil) compared to the other oils. The
systems. The total flavanoid contents in the seven cold- major tocopherol in the seven cold-pressed flaxseed oils
pressed flaxseed oils are lower than those found in whole was in the g form. g-Tocopherol was the only tocopherol
flaxseeds. This is due to the hydrophilic nature of found in WB and EBN and constituted 95.39–95.93% of
flavanoids, they are not effectively extracted with the oil. the total tocopherols in the other flaxseed oils with the
Total flavanoid content of flaxseeds as reported by Oomah exception of OSELO (55.15% of the total tocopherols).
et al. (1996) ranged from 30.2 to 83.5 mg/100 g. MEL and The b- and d-tocopherol were not detected in the seven
OSELC had the highest flavanoid contents among the cold-pressed flaxseed oils. As far as the authors are aware,
flaxseed oils. there is no report available on the occurrence of b-
The phenolic acid family is composed of the cinnamic tocopherol in flaxseed or flaxseed oil. Oomah et al. (1997)
(C6–C3) and the benzoic (C6–C1) acid derivatives, char- reported the presence of d-tocopherol in flaxseed but
acterized by containing a benzene ring substituted with one at very low levels (0.17–0.30 mg/100 g of seed) and
or more hydroxyl or methoxy groups and a carboxylic Velasco and Goffman (2000) reported the occurrence of
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Table 4
Tocopherol and plastochromanol-8 content of flaxseed oils (mg/100 g of oil)

a-Tocopherol g-Tocopherol Plastochromanol-8 Total tocopherols+plastochromanol-8

WB 0.00c 15.0070.17a 3.4870.14c 18.4870.31b


MEL 0.5170.19b 10.5670.83e 4.2870.49b 15.3571.51c
OSELC 0.5470.17b 12.8570.42bc 4.6770.26b 18.0770.85b
OSELO 9.1170.30a 11.2170.79de 4.1570.15b 24.4771.24b
FO 0.5570.14b 12.0771.01bcd 5.5370.26a 18.1571.41b
EBN 0.0070.00c 13.2970.60b 3.4270.64c 16.7171.25bc
HEA 0.5070.16b 11.9470.54cd 3.3770.37c 15.8171.07c

Values are means7standard deviations of three (n ¼ 3) measurements.


abc
Values with different superscript letters within a column indicate significant difference at po0.05.

Table 5
CIELAB L* a* b* value# of flaxseed oils

L* a* b*

WB 63.2470.01c 6.2370.02d 99.6870.27a


MEL 63.3970.01b 3.2870.01g 91.0870.22e
OSELC 63.7170.01a 4.5570.02f 94.8070.15d
OSELO 62.4870.01d 6.1370.02e 97.9970.15b
FO 60.8570.02f 7.6370.03b 96.8070.08c
EBN 62.3670.04e 7.5470.04c 99.8070.18a
HEA 60.0570.01g 9.5670.02a 97.7470.15b
#
L* designates the lightness of the sample, 100 ¼ white, 0 ¼ black; a* indicates redness when positive, greenness when negative; b* indicates yellowness
when positive, blueness when negative.
Values are means7standard deviations of three (n ¼ 3) measurements.
abcdefg
Values with different superscript letters within a column indicate significant difference at po0.05.

d-tocopherol at 0.0–0.3 mg/100 g of seed in 288 accessions respectively (Fig. 1). The peroxide value of oil is an
of the genus Linum. The plastochromanol-8 content found empirical measure of oxidation that is useful for samples
in the seven cold-pressed flaxseed oils was in accordance that are oxidized to relatively low levels (peroxide values of
with the reported values (1.7–5.4 mg/100 g of seed) of less than 50), and under conditions sufficiently mild so that
Velasco and Goffman (2000) but lower than that (22.3 mg/ hydroperoxides are not markedly decomposed. During
100 g) of linseed oil reported by Olejnik et al. (1997). These autoxidation, the peroxide value of oil reaches a maximum
differences may be due to the differences in the variety and followed by a decrease at more advanced stages varying
origin of the investigated samples. Olejnik et al. (1997) also according to the fatty acid composition of the oil and the
investigated the antioxidative properties of plastochroma- conditions of oxidation (Frankel, 2005).
nol-8 and found that it was a better natural antioxidant The p-anisidine test provides useful information on non-
than a-tocopherol in inhibiting the autoxidation of a model volatile carbonyl compounds formed in oils during
system in which lard was the substrate. Table 5 shows the processing and is often used to detect secondary oxidation
CIELAB L* a* b* color values of the seven cold-pressed products. Good quality oil should have a p-anisidine value
flaxseed oils. Significant differences were found between of less than two (Subramanian et al., 2000). The p-anisidine
the L*, a* and b* values of the oils (po0.05). There are values of the seven cold-pressed flaxseed oils varied
no color standards for cold-pressed flaxseed oils and the between 0.36 and 0.74 with MEL, OSELO and FO at the
L* a* b* measurements could thus be used for color higher end (Fig. 2). The Totox value (anisidine value+2 
classification. peroxide value) is used as an empirical measure of the
Figs. 1–7 show the quality characteristics of the seven precursor non-volatile carbonyls present in processed oils
cold-pressed flaxseed oils. Although the age of the oil is an plus any further oxidation products developed after
important factor for monitoring the quality of the oil, it is storage. Good-quality oil should have a Totox value of
not known here and could not be used for comparison. The less than four (Frankel, 2005). Fig. 3 shows that MEL, FO
peroxide values of all the cold-pressed flaxseed oils were and HEA have exceeded the Totox value for good-quality
well within the limit of up to 10 milliequivalents peroxide/ oil. All the other flaxseed oils, however, have Totox values
kg of oil and 15 milliequivalents peroxide/kg of oil under less than three. These Totox value results were largely
the New Zealand Food Regulations (1984) for edible fats derived from the peroxide values and suggest that MEL,
and oils, and the Codex Alimentarius Commission (1999) FO and HEA might undergo further oxidative degradation
standard for virgin oils and cold-pressed fats and oils, upon storage.
ARTICLE IN PRESS
208 W.-S. Choo et al. / Journal of Food Composition and Analysis 20 (2007) 202–211

18.00

15.00

Peroxide value (milliequivalent


12.00

peroxide/kg sample)
9.00

6.00

3.00

0.00
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils
New Zealand Food Regulations (1984)
Codex Alimentarius Commission (1999)
maximum thresholds

Fig. 1. Peroxide values of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements.

2.00

1.60
p-anisidine value (unit)

1.20

0.80

0.40

0.00
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils
Maximum threshold for p-anisidine
value by Subramanian et al. (2000)

Fig. 2. p-Anisidine values of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements.

7.00

6.00

5.00
Totox value (unit)

4.00

3.00

2.00

1.00

0.00
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils
Maximum threshold for Totox value
by Frankel (2005)

Fig. 3. Totox values of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements.
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W.-S. Choo et al. / Journal of Food Composition and Analysis 20 (2007) 202–211 209

0.18

0.15

% conjugated dienoic acid


0.12

0.09

0.06

0.03

0.00
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils

Fig. 4. Conjugated dienoic acids of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements. Note: Standard deviation of
percent conjugated dienoic acid of FO is zero.

2.8

2.4
Specific extinction (unit)

2.0

1.6

1.2

0.8

0.4

0.0
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils
232nm 270nm

Fig. 5. Specific extinction at 232 and 270 nm of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements. Note: Standard
deviation of specific extinction at 232nm of HEA is zero.

4.50
Acid value (mg KOH / g of sample)

4.00
3.50
3.00
2.50
2.00
1.50
1.00
0.50
0.00
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils

New Zealand Food Regulation (1984) & Codex


Alimentarius Commission (1999) maximum thresholds

Fig. 6. Acid values of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements.
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210 W.-S. Choo et al. / Journal of Food Composition and Analysis 20 (2007) 202–211

5.00

Food oil sensor readings (unit)


4.00

3.00

2.00

1.00

0.00
WB MEL OSELC OSELO FO EBN HEA
Flaxseed oils
Limit to discard the oil by
Gertz (2000)

Fig. 7. Food oil sensor readings of flaxseed oils. Values are means7standard deviations of three (n ¼ 3) measurements.

The conjugated diene hydroperoxides produced from pressed flaxseed oils were oils that have not undergone any
polyunsaturated lipids can be determined quantitatively by heat treatment, the FOS readings obtained were considered
their strong absorption maximum at 234 nm and their relatively high and this was due to calibration of the food
measurement is a sensitive method to follow the early oil sensor using the reference oil given by the manufacturer.
stages of lipid oxidation under conditions in which Gertz (2000) reported that FOS readings are strongly
hydroperoxides undergo little or no decomposition influenced by the type of oil and traces of salts, water and
(Frankel, 2005). Fig. 4 shows the percent of conjugated minerals in the oil. Middle- and long-chain fats and oils
dienoic acids of the seven cold-pressed flaxseed oils. These were found to have higher FOS readings.
results were in accordance with the percent of conjugated
dienes (0.08–0.16%) found by Zheng et al. (2003) for
organic oil obtained from screw pressing of whole and 4. Conclusions
dehulled flaxseed.
The specific extinction at 232 and 270 nm of the seven The results of this study showed that the seven cold-
cold-pressed flaxseed oils is shown in Fig. 5. The results of pressed flaxseed oils sold in New Zealand were quite similar
this test compare well with the peroxide values and percent in their physicochemical characteristics, with only a few
of conjugated dienoic acid. These were also in accordance significant variations. WB, OSELC, OSELO and EBN
with Reed et al. (2001) who reported that peroxide values passed all the quality tests according to the limit or
were more likely to be under the threshold value than UV maximum threshold of the above-mentioned regulations
absorbances. Fig. 6 shows that the acid values of the seven and literature. The characteristics of each flaxseed oil in
cold-pressed flaxseed oils were well within the limit of terms of its fatty acid composition, chlorophyll pigments,
4.0 mg KOH/g of oil under the New Zealand Food tocopherol and plastochromanol-8 contents may play
Regulation (1984) for virgin fats and oils, and Codex significant and/or synergistic roles in the quality of the
Alimentarius Commission (1999) for virgin oils and cold- oil. Total phenolic acids and flavanoids of the flaxseed oils
pressed fats and oils. These acid value measurements appear not to have much influence on the quality of the
correlated well with the free fatty acid measurements oils, probably due to their hydrophilic nature. It should be
shown in Table 3. noted that the influence of processing, packaging and age
Dielectric measurements were undertaken with a food oil of the oils were not able to be taken into considerations on
sensor which was calibrated with a reference oil 0.00 from the quality of the oils. Noting the increasingly popularity of
the manufacturer. The dielectric measurement changes flaxseed oil as a source on n-3 fatty acids, this study present
along with the quantity of polar components in each oil. a view of the characteristic and quality of cold-pressed
Increasing quantity of polar components indicates the flaxseed oils in New Zealand and could also serve as a
decreasing quality of the oil. According to Melton et al. starting point for developing quality standards since there
(1994), total polar components in fresh unused oil includes are no specifications available for flaxseed oil.
sterols, tocopherols, mono-and diglycerides, free fatty acids
and other oil-soluble components that are more polar than
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