Journal of the Science of Food and Agriculture J Sci Food Agric 84:1759–1764 (online: 2004)

DOI: 10.1002/jsfa.1877

Determination of high molecular mass

polycyclic aromatic hydrocarbons in refined
olive pomace and other vegetable oils
Wenceslao Moreda,∗ Rafael Rodrı́guez-Acuña, Marı́a del Carmen Pérez-Camino
and Arturo Cert
Instituto de la Grasa (CSIC), Avda Padre Garcı́a Tejero, 4, E-41012, Seville, Spain

Abstract: A new and simple method has been developed for determining high molecular mass polycyclic
aromatic hydrocarbons (PAHs) in refined olive pomace, and other vegetable oils from an initial sample
of 0.25 g. The hydrocarbon fraction is isolated by solid-phase extraction (SPE) on silica gel using
hexane as eluent. The fraction is evaporated to reduced volume and cleaned-up by SPE on an amino
phase eluting with toluene. The evaporated residue, dissolved in acetonitrile, is analyzed by reverse-
phase high-performance liquid chromatography with fluorescence detector using programmed excitation
and emission wavelengths. The benzo(e)pyrene is determined together with other usual heavy PAHs.
Interferences due to squalene and other hydrocarbons are minimized. Recoveries were greater than 80%
and detection limits ranged from 0.01 to 0.2 µg kg−1 . The method was validated using certified oil samples
and was applied to various vegetable oils.
 2004 Society of Chemical Industry

Keywords: heavy polycyclic aromatic hydrocarbon; benzo(e)pyrene; refined olive pomace oil; olive oil; vegetable
oil; analytical determination

INTRODUCTION important factor of the contamination rate is the

Polycyclic aromatic hydrocarbons (PAHs) are a
group of contaminants that occurs widely in the
environment as a result of incomplete combustion
of organic matter. Due to the wide distribution of
PAHs in the environment and their lipophilic nature,
edible vegetable oils can be contaminated with these
substances. Different routes of PAHs contamination
in vegetable oils have been suggested. The drying
process of the raw matter is usually responsible for
major PAHs contamination of some edible oils such
as sunflower, soybean and palm oils.1 Other sources
of contamination includes air pollution with dust
containing particles of pyrosynthesized PAHs that may
contaminate the plants or the raw material and hence
the final product.2,3
Significant contamination with PAHs has been
detected in crude olive pomace oil, known also as
olive residue oil. The contamination occurs mainly
during the drying of the olive pomace prior to the
solvent extraction process to obtain the residual oil
(1–7%). The olive pomace is dried by direct contact
with combustion fumes; therefore the extent of the
PAHs contamination depends on the type of fuel-gas,
or fuel-oil, and the solid residue from the solvent
extraction—used to dry the olive pomace. Another
humidity in the olive pomace since it affects the expo-
sure time necessary to achieve the water elimination.
There are two types of olive pomace, depending on the
process in the olive oil extraction: one with a water con-
tent of 30–40%, coming from crushed olives processed
by press or continuous centrifugation in three-phase
mode, and the other, with a water content of 70–80%,
coming from continuous centrifugation in two-phase
mode. A more aggressive drying is needed for the latter
type and consequently higher PAHs levels are usually
detected in the crude oils obtained from it.4
The oil obtained from the olive pomace cannot be
used directly for human consumption, but requires
refining to remove unwanted minor components
and undesirable organoleptic properties. This process
normally involves degumming, neutralization, partial
elimination of waxes, decolouration with activated
clays and deodourization. The decolouration step has
been amended to include the use of activated carbon
together with activated clays, which reduces signifi-
cantly the levels of PAHs in the oil.5,6 Olive oils contain
high amounts of squalene (800–8000 mg kg−1 ).7 The
decolouration step performed in crude oils during the
refining process partially isomerizes the squalene and
decomposes the steroidal alcohols, yielding a great

∗ Correspondence to: Wenceslao Moreda, Instituto de la Grasa (CSIC), Padre Garcia Tejero, 4, E-41012-Sevilla, Spain
E-mail: wmoreda@ig.csic.es
Contract/grant sponsor: Junta de Andalucia; contract/grant number: CAO01-005
(Received 4 November 2003; revised version received 7 April 2004; accepted 7 April 2004)
Published online 4 August 2004
 2004 Society of Chemical Industry. J Sci Food Agric 0022–5142/2004/$30.00 1759
W Moreda et al
number of unsaturated hydrocarbons with cyclic moi-
eties which have polarities similar to that of PAHs.7
There are, at the moment, no established limits val-
ues for any PAHs in edible vegetable oils in European
legislation, although several countries have adopted
limits for such compounds, either for a variable
number of PAHs or specifically for benzo(a)pyrene.
In particular, Spain has produced legislation, noti-
fied to the European Commission, which establishes
limiting values for high molecular mass PAHs in
olive pomace oil (Order 14 558 of 25 of July of
2001).8 This order establishes the maximum limits
for the following eight PAHs: benzo(a)pyrene (BaP),
benzo(e)pyrene (BeP), benzo(a)anthracene (BaA),
benzo(b)fluoranthene (BbFA), benzo(k)fluoranthene
(BkFA), dibenzo(a,h)anthracene (DBahA), benzo
(g,h,i)perilene (BghiP) and indeno(1,2,3-c,d)pyrene
(IP). The concentration of each PAH shall not exceed
2 µg kg−1 oil and the sum shall not exceed 5 µg kg−1 .
The order states also that the analysis should be under-
taken using a duly validated method.
Several methods for extraction and clean-up
of the PAHs fraction from fats and oils have
been described. Nowadays the isolation is per-
formed by HPLC on electron acceptor station-
ary phases (tetrachlorophthalimidopropyl-modified
silica),9 by column chromatography on alumina10
or silica gel,11 or by preparative size-exclusion liq-
uid chromatography.12 Although in some methods
the fraction is directly analyzed, a clean-up of the
extracts is needed to separate PAHs from numerous
organic compounds that interfere with the final deter-
mination. This purification is performed using column
chromatography, either on silica-gel,13,14 Florisil15 or
XAD-2 resin.16
The quantification of PAHs is usually performed
on the extract by reverse-phase HPLC in combi-
nation with fluorescence detection.1,5,14 The avail-
ability of special reverse stationary phases increases
resolution,9,17 and in conjunction with selective
wavelength-programmed fluorescence detection pro-
vide a rapid and sensitive method for PAHs determi-
nation.
The analysis has also been performed by GC on
capillary columns (100% dimethylpolysiloxane) using
an FID detector.18 Because of the lack of selectivity of
this detector, identification of chromatographic peaks
has been carried out by mass spectrometry.2,13 The
GC methods require significant amounts of sample,
although the on-line HPLC–GC-MS system allows,
in one step, the analysis of PAH in vegetable oils with
high selectivity and sensitivity.19
For determining benzo(a)pyrene in oils, there is
a standardized method based on the isolation of
the PAHs fraction by column chromatography on
alumina and analysis by HPLC with fluorescence
detector.10,20 For determining various the PAHs, a
very complicated method21 using several solid phase
extractions (SPE) and concentration steps is under
examination. The preliminary results indicates that the
1760
method is not applicable to refined olive pomace oils
because of the interferences by different compounds in
the HPLC analysis.22 References on the determination
of benzo(e)pyrene in vegetable oils by HPLC with
fluorescence detector (FLD) have not been found.
The objective of this paper was to develop and
optimize a simple analytical method for quantifying
heavy PAHs in refined olive pomace, olive and
other vegetable oils that fulfill the Spanish legislation,
and that can be easily carried out by oil industries
and official organisms to control the PAHs levels
in vegetable oils. The method consists in the
isolation of the hydrocarbon fraction and clean-up of
PAHs fraction using two SPE steps, and subsequent
analysis by reverse-phase HPLC with a programmable
wavelength fluorescent detector. The method has been
validated using certified oil samples and applied to
various types of vegetable oils. The precision and
limits of quantitation and determination were also
calculated.
EXPERIMENTAL
Samples
Samples of refined olive pomace oil obtained from
various Spanish refining industries were used to
develop and optimize the method. Virgin olive, olive
(virgin and refined mixture) and refined sunflower oils
were obtained from the market.
In order to validate the method, two certified
reference materials from BCR/IRMM (Brussels,
Belgium) were used. A highly refined coconut oil
(CRM 459) which was used as blank (certified values
of PAHs: <0.9 ng g−1 of PY, <0.6 ng g−1 of CHR,
<0.2 ng g−1 of BkFA, <0.3 ng g−1 of BaP, <0.2 ng g−1
of BghiP, <0.2 ng g−1 of IP) and a coconut oil (CRM
458) obtained by spiking a highly refined coconut oil
with respective PAHs in the lower ng g−1 possible
to validate the method (certified values of PAHs:
9.4 ng g−1 of PY, 4.9 ng g−1 of CHR, 1.87 ng g−1
of BkFA, 0.93 ng g−1 of BaP, 0.97 ng g−1 of BghiP,
1.00 ng g−1 of IP).
Materials and reagents
For the chromatographic analysis, acetonitrile HPLC
super-purity solvent 190 (ROMIL, Cambridge, UK),
and water purified with a Milli-Q system (Millipore,
Bedford, MA, USA) were used. For the clean-up
procedure, we used Si and NH2 Bondesil adsorbents
(Varian, California, USA), n-hexane and toluene
Uvasol grade (Merck, Darmstadt, Germany), and
alkane mixture of boiling point 65–70 ◦ C reagent
grade (Scharlau, Barcelona, Spain) distilled using a
Vigreux column.
Individual standard PAHs were obtained from Dr
Ehrenstorfer GmbH (Augsburg, Germany) at con-
centrations of 10 ng µl−1 : BaA, CHR, BeP, BbFA,
BkFA, BaP, DBahA, BghiP and IP in acetoni-
trile and benzo(b)crysene (BbC) in cyclohexane. A
stock solution containing: BaA 0.50 µg ml−1 , CHR
J Sci Food Agric 84:1759–1764 (online: 2004)

0.50 µg ml−1 , BeP 1.0 µg ml−1 , BbFA 0.50 µg ml−1 ,
BkFA 0.125 µg ml−1 , BaP 0.25 µg ml−1 , DBahA
0.25 µg ml−1 , BghiP 0.50 µg ml−1 and IP 1.75 µg ml−1
of the PAHs was prepared in acetonitrile and stored
at 4 ◦ C in darkness. A 0.5 ng ml−1 solution of BbC in
cyclohexane was used as internal standard solution.
The different calibration solutions were prepared by
appropriate dilutions of the stock solutions. The stock
solutions were stable almost for two months.
Apparatus
The HPLC equipment was composed of a vacuum
degasser for the mobile phase solvents Gastorr
154 (Flom, Japan), an auto-sampler System Gold
508, binary pumping unit System Gold 126, a
Mistral peltier column thermostat unit (Beckman-
Coulter, Fullerton, CA, USA) and a programmable
fluorescence detector LAChrom L-7485 (Hitachi-
Merck, Japan). A reverse-phase C-18 HPLC column
(250 × 4.6 mm ID) packed with Inertsil ODS-P
(5-µm particle size) (GL Sciences Inc, Tokyo,
Japan) was used together with a reverse-phase C-18
high-performance guard column (10 × 2.1 mm ID)
(5-µm particle size) packed with TP-201 (Vydac, CA,
USA). The data was processed using 32 karat Gold
acquisition software (Beckman-Coulter, Fullerton,
CA, USA).
Analytical procedure
Isolation of the hydrocarbon fraction
In a 25-ml conic flask, 250 mg of oil were weighed
(precision of 0.1 mg), then 2.5 ml of alkane mixture
and 200 µl of standard solution added (0.50 ng ml of
BbC in cyclohexane). The mixture was homogenized
by shaking. The silica column was prepared placing a
plug of cotton glass at the bottom of a glass column
(140 × 13 mm ID), then 2 g of silica were poured
onto the plug and the column was tapped to pack
it. The column was conditioned by passing 30 ml
of alkanes mixture without allowing it to dry. The
solution was charged onto the silica column and the
solution was pulled through under sometimes. The
flask was washed with two portions of 0.50 ml of
hexane that were also poured onto the column. The
column was eluted with an additional 5 ml of hexane
and the eluted fraction is discarded. The column was
then eluted with 30 ml of hexane and the fraction was
collected in a 50-ml conical flask. The solution was
evaporated in a rotary evaporator at room temperature
under vacuum to approximately 0.50-ml volume.
SPE clean-up
The amino-phase column was prepared placing a plug
of cotton glass at the bottom of a glass column
(140 × 13 mm ID), then 5 g of amino-phase were
poured onto the plug, and the column was tapped to
pack it. The column was placed into a vacuum system
and then conditioned by passing 30 ml of alkene
mixture without allowing it to dry. The concentrated
solution obtained from the silica column was charged
J Sci Food Agric 84:1759–1764 (online: 2004)
Heavy polycyclic aromatic hydrocarbons in olive pomace oils
onto the amino-phase column and the solution was
pulled through under vacuum. The flask was washed
with three portions of 200 µl each of the alkanes
mixture and the washings charged onto the column.
The column was then eluted under vacuum with 25 ml
of the alkanes mixture and the eluted solvent was
discarded. The column was then eluted under vacuum
with 15 ml of alkanes mixture/toluene (70:30) and the
fraction was collected in a 25-ml conic flask. The
solution was evaporated in a rotary evaporator under
vacuum just to dryness. The residue was almost free
of squalene as determined by GC.
HPLC analysis
The residue was re-dissolved in 50 µl of acetonitrile
by shaking. An aliquot of 20 µl was injected into the
HPLC using an auto-sampler with pick-up injection
mode to avoid cross-contamination. The HPLC
system was set up maintaining the column temperature
at 20 ◦ C and using a mixture of acetonitrile/water
as mobile phase at a flow rate of 1 ml min−1 . The
solvent gradient was as follows: from 0 to 3 min 85%
acetonitrile and then a linear gradient up to 100%
of acetonitrile in 34 min and hold for 28 min, then
from 65 to 66 min back to 85% of acetonitrile and
maintained for 4 min. The effluents were monitored
using the following wavelength programme: 0 to
22.2 min λex 270 nm and λem 385 nm (PAHs detected
BaA, CHR); 22.2 min λex 296 nm and λem 406 nm
(PAHs detected BeP, BbFA, BkFA, BaP, DBahA,
BghiP); 46.5 min λex 274 nm and λem 507 nm (PAH
detected IP); 52.2 min λex 290 nm and λem 427 nm
(PAH detected BbC). A good recovery of the internal
standard (BbC) indicates the complete elution of
heavy PAHs.
RESULTS AND DISCUSSION
Development of the PAHs isolation and clean-up
procedure
Refined olive pomace oil spiked with low concentra-
tions of PAHs was used for the development of the
method. The attempts to isolate the heavy PAHs from
the oil by column chromatography on alumina, silica-
gel and modified silica-gel (silver-loaded, amino, qua-
ternary amino and diol columns) using various eluting
solvents (hexane, cyclohexane, tert-butylmethyl ether
and mixtures of them) yielded PAHs fractions con-
taining considerable amounts of compounds that
interfered the with further analytical determination
by HPLC with fluorescence detector. The presence
of significant amounts of squalene was an additional
disadvantage since it gives an oily residue, insoluble in
acetonitrile that had to be dissolved in tetrahydrofuran
for the HPLC injection. This solution (50 µl) easily
evaporates resulting in a variable volume of solution.
Different qualities of eluting solvents were next
checked, because most of them contain hydrocarbons
that interfere in the analysis, requiring us to use hexane
and toluene of Uvasol quality and mixture of alkanes
1761
W Moreda et al

distilled through a Vigreux column. In the same way,
attempts were made using SPE cartridges but the
polymeric material of which the SPE cartridges are
made releases compounds interfering with BaA and
CHR into the solvent during the elution process; glass
columns were therefore used.
Isolation of the hydrocarbon fraction was optimized
using a column loaded with silica-gel phase. The
sample was eluted with n-hexane, rejecting the first
fraction that contains alkanes, alkenes and part of
the squalene. The second fraction contained the
remaining squalene and the heavy PAHs, while the
waxes and triacylglycerols remained in the column.
The extract was evaporated to reduced volume and
cleaned-up using another glass column filled with
other adsorbents, such as silica gel, silica gel loaded
with silver nitrate or amino-phases. The best results
were obtained using an amino phase, since this
adsorbent has affinity for the PAHs, retaining them
in the column.23 The non-aromatic hydrocarbons
and the light PAHs were eluted with an apolar
solvent (mixture of alkanes) while the heavy PAHs
remained on the stationary phase because of the major
interaction with the amino groups. The heavy PAHs
were desorbed by displacement with an aromatic
solvent (toluene). The extract obtained was then free
of significant interferences (Fig 1). The presence of the
0.05
2 5
Refined olive pomace
0.04
6 the smallest quantity of analyte that can be said to be
0.03
Volts
BbC peak assures the complete elution of the heavy
PAHs.
Development of HPLC analytical method
The HPLC method was developed and optimized
to fulfil the requirements of the Spanish Legislation,
since the Order states the determination of eight
PAHs, including BeP which elutes rather close to
BbFA. The best separations were obtained using
the reverse-phase Inertsil ODS-P as stationary phase
and water/acetonitrile as mobile phase. The elution
gradient was a compromise between peak separation
and run time. Sub-ambient oven temperature (20 ◦ C)
was needed to achieve a good separation between
BeP and BbFA peaks. For the fluorescence detection
of each compound, the excitation and emission
wavelengths that yield maximum response as well
as those used by other authors were tested. The
wavelengths chosen were a compromise between the
response of all PAH and the interfering compounds,
as well as acceptable separation between peaks that
allowed changes of excitation wavelengths.
Method validation
A stock solution containing amounts of each PAH
to give similar detection response was prepared.
Standards solutions were obtained by different
dilutions of this stock solution with acetonitrile. The
limit of detection (LOD) and the limit of quantitation
(LOQ) were calculated from standard solutions at
present with limit of confidence of 5% for LOD and the

3 10
0.02 1 4 7 8 smallest quantity of analyte that can be quantified with
9
a given level of confidence of 5% for LOQ.24 These
0.01
CRM 458 were calculated from the noise, and were taken as an
0.00 estimate of the blank standard deviation. The noise
0 5 10 15 20 25 30 35 40 45 50 55 60 and signal are measured and the LOD correspond to
Minutes the analyte amount for which the signal-to-noise ratio
of the peak height is equal to 3, and LOQ correspond
Figure 1. HPLC-FLD chromatogram profiles of refined olive pomace to a signal-to-noise ratio of 6.
oil and fortified refined coconut oil (certified CRM-458 sample):
The repeatability of the method was determined
(1) BaA; (2) CHR; (3) BeP; (4) BbFA; (5) BkFA; (6) BaP; (7) DBahA;
(8) BghiP; (9) IP; (10) BbC (IS). Experimental conditions as stated in
using refined olive pomace oil, and the results
the experimental section. PAHs concentrations are indicated in expressed by the relative standard deviation (RSD)
Tables 1 and 3. are shown together with the LOD and LOQ values

Table 1. Repeatability and limits of quantitation and determination values from within-laboratory determination of PAHs in refined olive pomace oil

Standard
HPLC peak Mean value (µg kg−1 ) deviation RSD (%) LOQ LOD
PAHs number (n = 6)a (n = 6)a (n = 6)a (µg kg−1 ) (µg kg−1 )

BaA 1 0.52 0.07 13.4 0.10 0.01

CHR 2 1.74 0.21 12.1 0.10 0.01
BeP 3 2.64 0.25 9.5 0.80 0.05
BbFA 4 1.03 0.11 10.7 0.40 0.03
BkFa 5 0.33 0.03 8.9 0.10 0.01
BaP 6 0.79 0.06 7.6 0.10 0.01
DBahA 7 0.05 < LOQ (0.2) 0.01 26.6 0.20 0.02
BghiP 8 0.48 0.04 7.6 0.40 0.05
IP 9 0.33 < LOQ (0.8) 0.09 26.0 0.80 0.20
a n = number of replicates.

1762 J Sci Food Agric 84:1759–1764 (online: 2004)

 Heavy polycyclic aromatic hydrocarbons in olive pomace oils

Table 2. Recoveries of PAHs added to strongly refined olive pomace oil

HPLC peak Fortification (A) Recovery (%) Fortification (B) Recovery (%)
PAHs number (µg kg−1 ) (n = 4)b (µg kg−1 ) (n = 4)

BaA 1 3.20 86.0 ± 4.3a 0.80 79.6 ± 3.6a

CHR 2 3.20 86.8 ± 5.6 0.80 84.4 ± 6.7
BeP 3 6.40 91.2 ± 5.7 1.60 88.3 ± 5.5
BbFA 4 3.20 94.7 ± 4.9 0.80 90.7 ± 5.8
BkFa 5 0.80 86.7 ± 5.2 0.20 79.5 ± 6.5
BaP 6 1.60 95.9 ± 6.1 0.40 91.3 ± 6.8
DBahA 7 1.60 88.5 ± 6.3 0.40 80.6 ± 6.8
BghiP 8 3.20 90.4 ± 6.5 0.80 81.2 ± 8.8
IP 9 11.20 88.0 ± 4.5 2.80 82.8 ± 3.3
a Standard deviation.
b n = number of replicates.

Table 3. Results obtained from applying the proposed analytical method to certified coconut oil samples

BCR 458 BCR 459

Mean value Certified Mean value

HPLC peak Theoretical Certified (µg kg−1 ) content (µg kg−1 )
PAHs number content (µg kg−1 ) content (µg kg−1 ) (n = 4)a (µg kg−1 ) (n = 4)a

CHR 2 4.99 4.90 4.47 ± 0.54 <0.60 0.12 ± 0.05

BkFa 5 2.00 1.87 1.89 ± 0.08 <0.20 <LOQ (0.1)
BaP 6 1.00 0.93 1.01 ± 0.06 <0.30 <LOQ (0.1)
BghiP 8 1.00 0.97 0.98 ± 0.11 <0.20 <LOQ (0.4)
IP 9 1.00 1.00 1.11 ± 0.14 <0.20 <LOD (0.20)
a n = number of replicates.

for the proposed method in Table 1. The proposed 0.06

2
method showed a good precision except for DBahA 0.05
1
and IP, because their concentrations were below the
0.04
limit of quantitation (LOQ).
The recoveries were determined using strongly 0.03
6
refined olive pomace oil, containing PAHs under 5
Volts

0.02
the LOD, which was fortified with the PAHs at two 34 10
7 8 9
levels. Table 2 show the recoveries obtained for the 0.01

two fortification levels, in which it can be seen that the 0.00

recoveries ranged between 80 and 96% with acceptable
-0.01
standard deviations. 0 5 10 15 20 25 30 35 40 45 50 55 60
Minutes
The method was validated using the certified
reference materials—BCR-459, a strongly refined Figure 2. HPLC-FLD chromatogram profile of refined high oleic
coconut oil, and, BCR-458, a coconut oil fortified sunflower oil: (1) BaA; (2) CHR; (3) BeP; (4) BbFA; (5) BkFA; (6) BaP;
with some PAHs. Table 3 shows the results obtained (7) DBahA; (8) BghiP; (9) IP; (10) BbC (IS). Experimental conditions as
using the proposed method; the precision of the stated in the experimental section, except that the final residue was
dissolved in 100 µl of acetonitrile instead of 50 µl. Concentrations are
determination is good, having an acceptable standard
shown in Table 4.
deviation in the BCR-458 and being, except for CHR,
below the LOQ and LOD in the blank (BCR-458).
Figure 1 shows also the HPLC chromatogram profile profile. The method can therefore be applied to refined
obtained from the BCR-458 oil using the proposed and non-refined vegetable oils regardless the content
method in which the correspondence to the PAHs of squalene and the process used.
determined in olive pomace oils is complete.
Some results from applying the proposed method
to various vegetable oils are shown in Table 4.
The HPLC profile obtained from refined high ACKNOWLEDGEMENT
oleic sunflower oil is depicted in Fig 2. The lack The authors thank to Mrs Rosario Goonzález
of baseline drift due to the absence of other Cordones and Mr Manuel Rodriguez Aguilar for
hydrocarbons coming from squalene isomerization technical assistance and to Junta de Andaluc ı́a for
and decomposition results in cleaner chromatographic financial support (Proyect CAO01-005).

J Sci Food Agric 84:1759–1764 (online: 2004) 1763

W Moreda et al

Table 4. PAHs concentrations found in various vegetable oils

Vegetable oils (µg kg−1 )

HPLC peak Refined olive Refined olive Refined olive Refined high oleic
PAHs number Virgin olive Olive Aa Olive Ba pomace A pomace B pomace C sunflower

BaA 1 0.10 0.28 0.36 <LOQb 0.14 0.11 5.17

CHR 2 0.38 0.84 1.23 0.14 0.26 0.43 11.95
BeP 3 NDc ND 1.31 <LOQ 0.80 1.98 4.40
BbFA 4 ND ND 0.96 <LOQ <LOQ <LOQ 4.21
BkFa 5 ND 0.16 0.22 <LOQ <LOQ 0.15 0.93
BaP 6 ND 0.27 0.26 ND <LOQ 0.34 2.18
DBahA 7 ND ND 0.32 ND <LOQ <LOQ 0.20
BghiP 8 ND 0.85 1.25 ND 0.40 0.62 1.66
IP 9 ND ND <LOQ ND ND <LOQ 1.20
Totald 0.10 1.56 4.68 0.00 1.34 3.2 19.95
a Mixture of virgin and refined olive oils.
b LOQ = limit of quantification.
c ND = not detected.
d According to Spanish legislation, sum of PAHs except CHR.

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