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FLAVOUR AND FRAGRANCE JOURNAL, VOL 8,Z-33 (1993)

On the Genuineness of Citrus Essential Oils. Part XLI. Italian


Bitter Orange Essential Oil: Composition and Detection of
Contamination and Additions of Oils and Terpenes of Sweet
Orange and of Lemon
Giovanni Dugo, Antonella Verzera, Ildefow Stagno d'Alcontres, Antonella Cotroneo and
Rita Ficarra
Dipartimento Farmaco-chimico, Facoltd di Farmacia, Universitd di Messina, 98100 Messina, Italy

The composition of the volatile fraction of Italian bitter orange essential oil, camed out by LC, HRGC and GC-
MS, is reported: 60 components have been identified. The results obtained are compared with those in the
literature for Italian and Spanish bitter orange oils.
Two methods are suggested which allows the detection of contamination or possible additions of terpenes and
oils of sweet orange and of lemon to genuine bitter orange oil. One is based upon the content of 6-3-carene and the
value of the ratios 6-3-carenelcamphene and 6-3-carenelterpinolene which permits the detection of the additions
of 5% of sweet orange terpenes and oils; the second is based upon the content of a-terpinene and the value of the
ratios a-terpinenelcamphene and a-terpinenelcis-B-ocimeneand allows the detection of the addition of even 3%
of lemon terpenes and oils.
KEY WORDS Citrus uuruntium L. Bitter orange essential oil Volatile fraction Commsition Adulteration
Sweet orange oil Sweet orange terpenes Lemon oil Lemon terpenes'

INTRODUCTION Therefore, we thought it useful to study the


composition of bitter orange essential oil, indus-
At present, the production of bitter orange essen- trially produced, and to develop a method which
tial oil is limited owing to the inconstancy of the allows the detection of contamination and of
demand on the national and international mar- additions of extraneous products.
kets leading to decreased cultivation. Spain,
Morocco and Tunisia produce large volumes of
bitter orange oils at lower prices than Italy. EXPERIMENTAL
The fruits used for the extraction of the essen-
tial oils are sometimes mixed with a small number The research has been camed out upon:
of sweet orange fruits and often the production
lines used are the same as those used for lemon -ten genuine samples of bitter orange oils, pro-
essential oil. duced by the usual industrial techniques (Pel-
It is possible, therefore, for bitter orange oil to atrice, Torchi and FMC)during the production
be contaminated by sweet orange and lemon season 1991/92; each sample represents more
essential oils. Moreover, sweet orange terpenes than 100 kg of essential oil;
and lemon terpenes could be deliberately added -eight laboratory prepared blends, obtained by
to bitter orange oil. the addition of sweet orange oils to genuine
Lawrence' and then Boelens2 have reviewed bitter orange oils in percentages varying from
the literature on the composition of the volatile 3% to 5 % ;
fraction of bitter orange oil. The composition of -eight laboratory prepared blends, obtained by
Italian bitter orange oil was studied by Boelens3 the addition of commercially available sweet
but the author does not report the number of the orange oil terpenes to genuine bitter orange
samples analysed nor the variability ranges for oils in percentages varying from 3% to 5%;
each component. -eight laboratory prepared blends, obtained by

0882-5734/93/010025~$09.50 Received 3 July 1992


0 1993 by John Wiley & Sons, Ltd. Accepted 24 August 1992
26 G.DUG0 E T A L.

the addition of lemon oils to genuine bitter ent classes of compounds on a neutral alumina
orange oils in percentages varying from 3% to column using the following experimental con-
5%; ditions: glass column (1.6cm i.d.; adsorbent,
-eight laboratory prepared blends, obtained by neutral alumina, grade I1 activity, 20g; sample,
the addition of commercially available lemon 100 pl of essential oil. Eluents: fraction 1 (hydro-
oil terpenes to genuine bitter orange oils in carbons), light petroleum (b.p. 30-50°C); frac-
percentages varying from 3% to 5%; tion 2 (esters), light petroleum: diethyl ether
(97:3 v:v); fraction 3 (carbonyl compounds), light
Each sample of oil has been analysed by GC on
petroleum: diethyl ether (80:20); fraction 4 (alco-
a Carlo Erba gas chromatograph 5160 Mega
Series, equipped with a Shimadzu data processor hols), diethyl ether. Each fraction was analysed
by GC using the same conditions as for each oil.
C-R3A using the following experimental con-
ditions, previously described for other citrus
essential glass capillary column, 25 m x
RESULTS
0.32mm i.d. coated with SE 52; column tempera-
ture, 60°C (8 minutes) to 100°C at 3"C/min, to
Composition of Bitter Orange Essential Oil
130°C at 2.5"C/min7to 180OC at 3"C/min; injector
and detector temperatures, 280°C; carrier gas, Figure 1 shows a chromatogram of the volatile
hydrogen, 0.40 kg/cm2; injection mode, split; de- fraction of bitter orange essential oil.
tector, FID. Sixty components were identified and, based on
The compounds were identified by retention the chromatographic behaviour on neutral alumina
time and by GC-MS using a Finnigan Mat ITD columns, the class to which some of the others
800 with a 25 m x 0.32mm i d . fused-silica capil- belong was determined. Table 1 reports the com-
lary column coated with SE 52; column tempera- position, as relative percentage of the areas of the
ture 60°C to 240°C at 3"C/min; ionizing voltage peaks, of the single components and of the classes
70 eV. of substances of bitter orange oils analysed. The
A bitter orange oil was fractionated into differ- same table shows the average value ( X ) , the

52
I

m N 4 m N
t
I,,
T i m e (minutam)
I.
N
N 4 m v
t
.
)
*

Fig. 1 . Chromatogram of a bitter orange essential oil. For identification of components see Table 1
ITALIAN B I T E R ORANGE ESSENTIAL OIL 27

standard deviation (s), the minimum and the Detection of Contamination and Additions of
maximum value for each parameter. The pro- Essential Oils and Terpenes of Sweet Orange
duction technology and period are indicated for Figure 2 compares the chromatogram of bitter
each sample. orange oil with those of the oil and the terpenes of
We can observe from the results reported in sweet orange. 8-3-Carene is present only as traces
Table 1 that the percentage content of monoter- in bitter orange oil, while in the oil and terpenes
pene hydrocarbons varies from 97.3% to 97.8%, of sweet orange it has a percentage of about
while sesquiterpene hydrocarbons have a percen- o.1%.6
tage of about 0.2%. Oxygenated compounds have It can be expected, therefore, as found with
a percentage between 1.8% and 2.2%. Esters are lemon6 and mandarin’ essential oils, that the 8-3-
the main oxygenated class; their content ranges carene content and the percentage ratios of the
from 0.8% to 1.4%; carbonyl compounds from latter in regard to other components is particularly
0.35% to 0.63% and alcohols from 0.33% to suited to indicate possible additions of these
0.46%. The main component of bitter orange extraneous products.
essential oil is limonene, its content being always In this case we have used the ratios 8-3-carene/
more than 93%. Among the minor monoterpene camphene and 8-3-carene/terpinolene.
hydrocarbons, only myrcene always exceeds 1%; Table 2 reports the 99% confidence limits for
its content ranges from 1.7% to l.8%, P-pinene the 8-3-carene content and for the ratios 6-3-
has a percentage of about 1% and a-pinene about carene/camphene and 6-3-carene/terpinolene,
0.5%. Linalyl acetate is the main oxygenated calculated on the basis of the average values and
compound and it represents the major part of the the standard deviations for genuine bitter orange
esters. Linalol is the main alcohol and octanal and oils, and the results obtained by the addition to
decanal the main carbonyl compounds. these of 3% and 5% of oils and of terpenes of
Our results on bitter orange oil agree with sweet orange.
those of Boelens3 with the exception of the con- As can be observed from the results reported in
tent of aliphatic aldehydes, in particular octanal, Table 2, only a few 3% blends show values higher
nonanal and decanal, for which Boelens gives than those of genuine oils, while all the blends
values approximately double those reported by containing 5% of the terpenes and of the oils of
us. In addition the content of limonene is slightly sweet orange show considerably higher values
higher in our samples. for the three parameters considered than those
Further, Boelens3 reported two decadienals, registered for the genuine bitter orange oils.
tridecanal, myrtenal, geraniol, p-menthane Even though a low amount of orange terpenes
acetate, carvone and p-sinensal which we have can always be detected, its percentage cannot be
not detected in our samples. We have detected accurately determined, because it depends upon
the presence of hexanol, 83tarene, a-terpinene, thecomposition oftheproductsused fortheblends.
cis-P-ocimene, cis-sabinene hydrate, trans-
sabinene hydrate, isopulegol, borneol, nonanol,
piperitone, nonyl acetate, a-terpenyl acetate, Detection of Contamination and Additions of Oils
citronellyl acetate, (3-sesquiphellandrene, trans- and Terpenes of Lemon
nerolidol and, &,trans-farnesol, which were not
reported by Boelens. Figure 3 compares the chromatogram of a bitter
With respect to the composition of the sesquiter- orange oil with those of a lemon oil and the terpenes
pene hydrocarbons fraction, it is not possible to of lemon oil.
make a comparison with our results because As we can observe from the figure, a-terpinene
Boelens reports only the total amount of these is present only as traces in bitter orange oil while
components. it has a percentage of approximate9 0.2% in
The sesquiterpene fraction of our bitter orange lemon oils and their terpene fraction.
oils is different from that of Spanish oils;*in fact we Therefore, the content of a-terpinene and the
have identified trans-P-bergamotene, p-santalene, percentage ratios of the latter in regard to other
germacrene-B and P-sesquiphellandrene which components can give useful indications for the
are not reported in the Spanish oils, while detection of possible additions of lemon products.
Boelens found 8-elemene and p-elemene which Our method uses the ratios a-terpinenej
are lacking in our samples. camphene and a-terpinenelcis-P-ocimene.
Table 1. Composition in single components and in classes of substances of the genuine bitter orange essential oils

No. Component Pelatrice Pelatrice Torchi FMC Pelatrice Pelatrice Pelatrice Pelatrice Pelatrice Pelatrice Min. Max. X s
Oct. 30 Nov. 8 Nov. 8 Nov. 27 Dec. 10 Jan. 13 Jan. 17 Jan. 17 Jan. 19 Jan. 21

1 Hexanol 0.003 0.001 0.001 0.001 0.001 0.001 0.001 - 0.001 0.001 O.OO0 0.003 0.001 0.001
2 a-Thujene 0.008 0.009 0.007 0.007 0.007 0.004 0.004 0.004 0.005 0.006 0.004 0.009 0.006 0.002
3 a-Pinene 0.565 0.574 0.585 0.562 0.547 0.521 0.558 0.555 0.581 0.584 0.521 0.585 0.563 0.019
4 Camphene 0.007 0.007 0.007 0.006 0.006 0.005 0.007 0.007 0.007 0.006 0.005 0.007 0.007 0.001
5 Sabinene 0.267 0.269 0.270 0.263 0.263 0.452 0.313 0.314 0.320 0.418 0.263 0.452 0.315 0.064
6 &Pinene 0.931 0.935 0.940 0.791 0.867 0.634 1.032 1.023 1.281 0.963 0.634 1.281 0.940 0.159 2
7 Myrcene 1.843 1.816 1.7% 1.832 1 .m 1.788 1.705 1.764 1.750 1.797 1.705 1.843 1.789 0.039 Q
8 Octanal 0.132 0.137 0.141 0.147 0. I31 0.191 0.109 0.I07 0.106 0.150 0.106 0.191 0.135 0.024 0
9 a-Phellandrene 0.056 0.059 0.061 0.063 0.056 0.082 0.047 0.046 0.045 0.064 0.045 0.082 0.058 0.010 3
10 S3-Carene 0.003 0.002 0.002 0.004 0.002 0.005 0.002 0.001 0.001 0.004 0.001 0.005 0.003 0.001
11 a-Terpinene 0.002 0.002 0.003 0.005 0.002 0.001 0.001 0.001 0.001 0.001 0.001 0.005 0.002 0.001 p
12 pCymene + Limonene 93.318 93.520 93.553 93.861 93.818 93.667 93.793 93.312 93.200 93.584 93.200 93.861 93.563 0.218 .
13 cis+-Ocimene 0.013 0.014 0.013 0.011 0.012 0.009 0.006 0.006 0.006 0.007 0.006 0.014 0.010 0.003
14 fram-&Ocimene 0.375 0.371 0.382 0.340 0.342 0.187 0.273 0.247 0.283 0.279 0.187 0.382 0.308 0.061
15 7-Terpinene 0.100 0.127 0.067 0.090 0.074 0.012 0.008 0.007 0.014 0.058 0.007 0.127 0.056 0.041
16 cirSabinene hydrate 0.004 0.002 0.003 0.003 0.003 0.005 0.002 0.002 0.002 0.008 0.002 0.008 0.003 0.002
17 Oaanol 0.004 0.001 0.003 0.004 0.005 0.005 0.009 0.014 0.001 0.001 0.001 0.014 0.005 0.004
18 Terpinolene 0.008 0.009 0.007 0.010 0.010 0.006 0.004 0.004 0.004 0.007 0.004 0.010 0.007 0.002
19 &am-Sabinene hydrate 0.001 0.001 - 0.001 - 0.001 0.001 0.001 0.001 0.001 o.oO0 0.001 0.001 o.Oo0
20 Linalol 0.333 0.267 0.268 0.267 0.204 0.312 0.258 0.275 0.199 0.316 0.199 0.333 0.270 0.042
21 Nonanal 0.033 0.034 0.035 0.031 0.030 0.036 0.015 0.017 0.016 0.026 0.015 0.036 0.027 0.008
22 cis-Limonene oxide 0.009 0.008 0.010 0.007 0.006 0.001 0.001 0.001 0.001 0.001 0.001 0.010 0.005 0.004
23 &am-Limonene oxide 0.006 0.004 0.006 0.005 0.005 0.001 0.002 0.001 0.001 0.001 0.001 0.006 0.003 0.002
24 Isopulegol 0.003 0.001 0.001 0.004 0.006 0.006 0.003 0.004 0.002 0.005 0.001 0.006 0.003 0.002
25 Citronella1 0.004 0.004 0.004 0.005 0.005 0.015 0.002 0.003 0.002 0.008 0.002 0.015 0.005 0.004
26 Borneol 0.002 0.001 0.005 0.001 0.002 0.001 0.001 0.001 0.001 0.001 0.001 0.005 0.002 0.001
27 Nonanol 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 o.Oo0
28 Terpinen-Qol 0.008 0.005 0.007 0.006 0.006 0.001 0.002 0.004 0.001 0.001 0.001 0.00s 0.004 0.003
29 a-Terpineol 0.050 0.040 0.030 0.037 0.059 0.036 0.043 0.045 0.037 0.039 0.030 0.059 0.042 0.008
30 Deanal 0.106 0.106 0.114 0.111 0.117 0.194 0.110 0.118 0.111 0.144 0.106 0.194 0.123 0.026
31 Octyl acetate 0.034 0.033 0.035 0.032 0.035 0.032 0.042 0.050 0.048 0.035 0.032 0.050 0.038 0.006
32 N e d Citronellol
+ 0.006 0.004 0.007 0.005 0.005 0.004 0.001 0.004 0.001 0.001 0.001 0.007 0.004 0.002
33 Ncral 0.053 0.048 0.052 0.050 0.055 0.049 0.034 0.038 0.032 0.044 0.032 0.055 0.045 0.008
34 Piperitone 0.003 0.001 0.001 0.001 0.002 0.001 0.003 0.001 0.002 0.001 0.001 0.003 0.002 0.001
35 Linalyl acetate 0.940 0.840 0.924 0.757 0.819 0.642 1.033 1.173 1.047 0.765 0.642 1.173 0.894 0.152
36 Geranial 0.098 0.086 0.086 0.084 0.079 0.083 0.048 0.054 0.051 0.066 0.048 0.098 0.074 0.017
37 Perillaldehyde 0.01 1 0.010 0.010 0.009 0.010 0.010 0.005 0.010 0.010 0.010 0.005 0.011 0.009 0.002
38 Undecanal 0.015 0.015 0.012 0.007 0.008 0.008 0.003 0.001 0.003 0.004 0.001 0.015 0.008 0.005
39 Nonyl acetate 0.003 0.001 0.001 0.002 0.004 0.008 0.001 0.003 0.003 0.004 0.001 0.008 0.003 0.002
40 Ester 0.005 0.017 0.024 0.026 0.028 0.010 0.013 0.012 0.013 0.012 0.005 0.028 0.016 0.007
41 a-Terpenyl acetate 0.006 0.006 0.007 0.005 0.007 0.005 0.007 0.005 0.006 0.004 0.004 0.007 0.006 0.001
42 Citronellyl acetate 0.008 0.008 0.009 0.008 0.009 0.006 0.005 0.006 0.006 0.005 0.005 0.009 0.007 0.001
43 Neryl acetate 0.018 0.018 0.019 0.022 0.024 0.016 0.018 0.022 0.023 0.018 0.016 0.024 0.m0.003
44 Geranyl acetate 0.111 0.105 0.110 0.110 0.114 0.075 0.081 0.099 0.101 0.079 0.075 0.114 0.098 0.014
45 Dodecanal 0.014 0.014 0.015 0.015 0.018 0.026 0.010 0.013 0.012 0.015 0.010 0.026 0.015 0.004
46 Decyl acetate 0.018 0.018 0.022 0.020 0.023 0.030 0.031 0.037 0.038 0.030 0.018 0.038 0.027 0.007
47 p-Caryophyllene 0.063 0.058 0.062 0.061 0.060 0.035 0.042 0.047 0.046 0.044 0.035 0.063 0.052 0.010
48 tram-p-Bergamotene 0.019 0.009 0.017 0.018 0.017 0.011 0.011 0.014 0.015 0.009 0.009 0.019 0.014 0.004
49 p-Humulene 0.009 0.008 0.009 0.009 0.009 0.006 0.007 0.005 0.004 0.006 0.004 0.009 0.007 0.002
50 0-Santalene 0.01 1 0.010 0.012 0.010 0.011 0.011 0.003 0.008 0.007 0.006 0.003 0.012 0.009 0.003
51 Carbonyl compound 0.013 0.012 0.013 0.013 0.015 0.013 0.007 0.011 0.012 0.009 0.007 0.015 0.012 0.002
52 Germacrene-D 0.134 0.115 0.125 0.111 0.115 0.087 0.089 0.102 0.108 0.095 0.087 0.134 0.108 0.014
53 Germacrene-B 0.011 0.009 0.01 1 0.010 0.010 0.008 0.007 0.009 0.008 0.007 0.007 0.011 0.009 0.001
54 PBisabolene 0.004 0.004 0.001 0.004 0.006 0.006 0.001 0.001 0.001 0.003 0.001 0.006 0.003 0.002
55 p-Sesquiphellandrene 0.009 0.008 0.010 0.01 1 0.012 0.008 0.07 0.009 0.008 0.008 0.007 0.012 0.009 0.001
56 bons-a-Nerolidol 0.045 0.047 0.054 0.057 0.064 0.062 0.062 0.081 0.083 0.062 0.045 0.083 0.062 0.012
57 Tetradesanal 0.002 0.001 0.003 0.001 0.003 0.001 0.001 0.001 0.001 0.001 0.001 0.003 0.002 0.001
58 cb,trans-Famesol 0.003 0.001 0.004 0.004 0.006 0.012 0.004 0.001 0.003 0.003 0.001 0.012 0.004 0.003
59 a-Sinensal 0.001 0.001 - 0.002 0.002 0.001 0.001 0.001 0.001 0.001 o.oO0 0.002 0.001 0.001
60 Nootkatone 0.002 0.001 - 0.002 0.002 0.001 0.001 0.001 0.001 0.001 o.oO0 0.002 0.001 0.001

Hydrocarbons 97.756 97.935 97.940 98.081 98.046 97.555 97.920 97.486 97.695 97.96097.486 98.079 97.836 0.195
Monoterpenes 97.4% 97.714 97.693 97.847 97.806 97.383 97.753 97.291 97.498 97.78297.291 97.845 97.625 0.185
Sesquiterpenes 0.260 0.221 0.247 0.234 0.240 0.172 0.167 0.195 0.197 0.178 0.167 0.260 0.211 0.032
Oxygenated compounds 2.089 1.887 2.018 1.847 1.896 1.897 1.959 2.202 1.978 1.872 1.847 2.202 1.964 0.106
Carbonyl compounds 0.487 0.470 0.486 0.478 0.477 0.629 0.349 0.376 0.360 0.480 0.349 0.629 0.459 0.078
Alcohols 0.459 0.371 0.381 0.387 0.357 0.442 0.379 0.419 0.333 0.440 0.333 0.459 0.397 0.039
Esters 1.143 1.046 1.151 0.982 1.063 0.825 1.231 1.407 1.285 0.952 0.825 1.407 1.108 0.163
30 G . DUG0 E T A L .

Table 2. Values for the 63-carene content, the 8-3-carenelcampheneand 63-carenelterpinolene ratios for
genuine bitter orange essential oils and for samples of bitter orange oils with 3% and 5% additions of sweet
orange oils and sweet orange terpenes

6-3-Carene 6-3-Carene/camphene 6-3-Carenelterpinolene

Bitter orange oil


x 0.003 0.424 0.389
S 0.001 0.259 0.189
99% confidence Min. 0.Ooo 0.Ooo 0.000
limits Max. 0.006 1.092 0.875
Bitter orange oils with sweet orange oils added
1.ooo 0.778
0.857 0.750
3% 1.286 0.900
0.714 0.500
1.500 1.Ooo
0.008 1.143 0.889
5% 0.012 1.714 1.091
10.007 1.Ooo 0.777
Bitter orange oils with sweet orange
1.Ooo 0.778
1.Ooo 1.Ooo
3%
0.857 0.857
0.857 0.750
1.375 1.Ooo
1.286 1.125
5%
1.125 0.900
1.111 1.Ooo

Table 3. Values for the a-terpinene content, the a-terpinenelcamphene and a-terpinene/ci.s-B-ocimeneratios
for genuine bitter orange essential oils and for samples of bitter orange oils with 3% and 5% additions of lemon
oils and of lemon terpenes

a-Terpinene a-Terpinenelcamphene a-Terpinenelcir-~-ocimene


Bitter orange oil
x 0.002 0.2% 0.266
S 0.001 0.201 0.107
99% confidence Min. 0.Ooo 0.Ooo 0.000
limits Max. 0.005 0.814 0.429
Bitter orange oils with lemon oils added
0.010 1.111 0.588
0.889 0.364
3%
1.Ooo 0.409
0.008 0.889 0.348
0.014 1.400 1.000
0.01 1 1.100 0.440
5%
0.013 1.300 0.619
0.010 1.111 0.526

*0.011 1.100 0.61 1


0.01 1
' 0.015 1.222 0.524
3%
1.250 0.555
0.014 1.273 0.538
'0.017 1.417 0.809
5% ' 0.017 1.700 0.809
0.020 1.538 0.714
-0.019 1.461 0.704
ITALIAN B I T E R ORANGE ESSENTIAL OIL 31

W E T ORAWCL OIL

L * - ? . e : l f

T h e (minut.8)
1,L
X
*

i
,

t
I

Fig. 2. Chromatograms of a bitter orange oil, of sweet orange oil terpenes and of sweet orange oil
32 0 . DUG0 ET AL.

i,
LEMON OIL

li. LEMON OIL TLRPEWES

L - f ~ z : z

T i m (minutom)
a a v t v

Fig. 3. Chromatograms of a bitter orange oil, of lemon oil terpenes and of a lemon oil
ITALIAN B I T E R ORANGE ESSENTIAL OIL 33

Table 3 reports the values of the a-terpinene (6OY0 and 40% research funds) and by National Re-
content and of the ratios a-terpinene/camphene search Council of Italy, Special Project 'Chimica Fine e
and a-teminene/ck-B-ocimene in genuine bitter
orange oiis and in the blends obtahed adding to
these 3% and 5% of terpenes and oils of lemon.
As can be observed from the results reported in
Table 3, all blends even those containing 3% of REFERENCES
lemon products, showed considerably higher
values than those registered for the genuine bitter 1. B. H.Lawrence, Perfwner & Flavorist, 5 , 5 5 (1982).
orange at least for two out of three parameters 2. M. H.Boelens, Perfumer & Fluvorist, 16, 17 (1991).
taken into account. 3. M. H.Boelens, and R. Jimenez, J. Ess. Oil Res., 1, 151
It is evident that our method allows the detec- (1989).
4. A. Cotroneo, G. Dugo, L. Favretto and L. Gabrielli
tion of even low amounts of oil and of terpenes Fawetto, 1. Chromarogr.,449, 183 (1988).
of lemon even though its percentage cannot be 5 . Giacomo Dugo, A. Cotroneo, A. Verzera, G. Dugo and
accurately determined for the same reason as G. Licandro, Flavour Frugr. J . , 5, 205 (1990).
mentioned for the addition of sweet orange oils A. Verzera, A. Cotroneo, G. Dugo and F. Salvo, Flavour
Frugr. J., 2 , 13 (1987).
and terpenes. 7. A. Cotroneo, Giacomo Dug0 and G. Dugo, Riv. Soc. It.
Sci. Alim., 16, 331 (1987).
Acknowledgements-This research was supported by 8. A Cotroneo, A. Verzera, G. Lamonica, G. Dugo and G.
'Minister0 dell'Universit8 e della Ricerca Scientifica' of Italy Licandro, Flavour Fragr. J . , 1, 69 (1 986).

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