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Journal of Food Engineering 90 (2009) 409413

Contents lists available at ScienceDirect

Journal of Food Engineering


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

Research Note

A new process for extraction of essential oil from Citrus peels: Microwave
hydrodiffusion and gravity
Nabil Bousbia a,b, Maryline Abert Vian c, Mohamed A. Ferhat a, Brahim Y. Meklati a, Farid Chemat c,*
a
Centre de Recherche Scientique et Technique en Analyses Physico-Chimiques, CRAPC, Alger, Algeria
b
Institut National Agronomique, El Harrach, Alger, Algeria
c
UMR A 408, Scurit et Qualit des Produits dOrigine Vgtale, INRA, Universit dAvignon et des Pays de Vaucluse, 84000 Avignon, France

a r t i c l e i n f o a b s t r a c t

Article history: Attention is drawn to the development of a new and green alternative technique for the extraction of
Received 15 January 2008 essential oil from citrus peels. The process uses the hydro-diffusion phenomenon generated by micro-
Received in revised form 30 May 2008 waves to extract essential oil from the inside to the outside of the biological material and gravity to col-
Accepted 18 June 2008
lect and separate them. The present apparatus permits fast and efcient extraction, reduces waste, avoids
Available online 3 July 2008
water and solvent consumption, and allows substantial energy savings.
2008 Elsevier Ltd. All rights reserved.
Keywords:
Microwave
Extraction
Hydro-diffusion
Essential oil
Citrus

1. Introduction of attention due to the increasing energy prices and the drive to re-
duce CO2 emissions. These shortcomings have led to considering
Citrus essential oils are the most widely used essential oils in the use of new techniques in the extraction of natural substances,
the world. They are obtained as by-products of the citrus process- which typically use less solvent and energy, such as supercritical
ing. They are used as aroma avor in many food products, includ- uid extraction, ultrasound extraction, the controlled pressure
ing alcoholic and non-alcoholic beverages, candy, gelatins, In drop process, and sub-critical water extraction. Researchers in
pharmaceutical industries they are employed as avoring agents many universities are working on novel techniques that could lead
to mask unpleasant tastes of drugs. In perfumery and cosmetic, to compact, safe, efcient, energy saving, and sustainable extrac-
they are used in many preparations. The traditional way to extract tion processes (Luque de Castro et al., 1999; Pollien et al., 1998;
essential oils is by cold pressing the citrus peels. The oil is present Reverchon, 1997; Vinatoru, 2001; Jimenez-Carmona et al., 1999;
in oil sacs or oil glands located at different depths in the peel and Rezzoug et al., 2000; Ganzler et al., 1986; Lucchesi et al., 2004).
the cuticles of the fruit. Peel and cuticle oils are removed mechan- In this study, a new and original process for the extraction of nat-
ically by cold pressing and since cold pressing yields a watery ural substances using microwave hydro-diffusion and gravity
emulsion, this emulsion is then centrifuged to separate out the (MHG) was designed and developed (Fig. 1). This green extraction
essential oil. Distillation is also used in some countries as an eco- process is an original combination of microwave heating and grav-
nomical way to recover the oils. During distillation, the Citrus peels ity working at atmospheric pressure. MHG was conceived for the
exposed to boiling water or steam, release their essential oils extraction of natural substances from different plant materials at
through evaporation. As steam and essential oil vapours are the laboratory and industrial scales. In this relatively simple meth-
condensed, both are collected and separated in a vessel od, the plant material is directly placed in a microwave reactor
traditionally called the Florentine ask (Guenther, 1948; Dugo without any added solvent or water. The internal heating of the
and Di Giacomo, 2002). in situ water within the plant material distends the plant cells and
The development of new separation techniques for the chemi- leads to rupture of the glands and cell receptacles. Heating under
cal, food and pharmaceutical industries has lately received a lot microwaves thus frees molecules of interest together with in situ
water. This physical phenomenon, known as hydro-diffusion, al-
lows the extract to diffuse outside the plant material and drop by
* Corresponding author. earth gravity out of the microwave reactor through the perforated
E-mail address: farid.chemat@univ-avignon.fr (F. Chemat). Pyrex disc. A heat exchanger outside the microwave oven cools

0260-8774/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2008.06.034
410 N. Bousbia et al. / Journal of Food Engineering 90 (2009) 409413

The potential of the green MHG technique has been investi-


gated for isolation of essential oil and compared with conventional
methods, hydro-distillation (HD) and cold pressing (CP), as the cur-
rent technique and commercial situation call for research about
new extracts and new extraction techniques. We have applied
MHG, HD and CP techniques to extract essential oil from citrus
peels. Belonging to the Rutaceae family, their essential oils are lo-
cated in lysigenous secretory reservoirs inside the avedo of the
fruit. Extraction yields and rates, essential oil compositions, and
energy consumption are compared.

2. Experimental

2.1. Plant material

In this study, citrus fruits were gathered from the same exper-
imental plantation Institut Technique de lArboriculture Fruitire
(I.T.A.F.), located in the Mitidja region 40 km south of Algiers (Bou-
farik, Algeria). The citrus fruits are: Eureka (Citrus limon L.), Villa
Frana (Citrus limon L.), lime (Citrus aurantifolia (Chrism.) Swing),
Marsh Seedless (Citrus paradisi L.), Tarocco (Citrus sinensis L.),
Valencia late (Citrus sinensis L.), Washington Naval (Citrus sinensis
L.), Tengelo Seminole (Citrus paradisi Macf.). Citrus fruits were
peeled to separate the external part of the lemon (avedo), giving
a yield of 20% (w/w) of the peel with respect to the whole fruit.
Fresh plant material was employed in all extractions.

2.2. Extraction apparatus and procedures

Hydro-distillation with a Clevenger-type apparatus was used to


extract 500 g of fresh citrus peels with 3 l of water for 3 h (until no
more essential oil was obtained). For cold pressing, essential oil
was collected from 1 kg of whole lemon fruit using an automated
cold pressing machine from Schwaub. The epidermis and oil glands
were lacerated by a needle, creating areas of compression in the
peel, surrounded by areas of lower pressure, across which the oil
owed to the exterior. The oil is carried down to a decantation
vessel in a stream of water, the emulsion being collected and then
separated by centrifugation. Microwave extrcation has been per-
formed in a Milestone microwave laboratory oven (Milestone
srl). In a typical procedure at atmospheric pressure, 500 g of fresh
citrus peels was heated using a xed microwave power 500 W for
15 min. The essential oil was collected, dried under anhydrous so-
dium sulphate and stored at 4 C until used. Extractions were per-
formed at least three times, and the mean values were reported.
The extraction apparatus are illustrated in Fig. 1.

2.3. Gas chromatography and gas chromatographymass


spectrometry identication

The essential oils were analyzed by gas chromatography cou-


pled to mass spectrometry (GCMS) (HewlettPackard computer-
ized system comprising a 6890 gas chromatograph coupled to a
5973A mass spectrometer) using two fused-silica-capillary col-
umns with different stationary phases. The non-polar column
was HP5MSTM (30 m  0.25 mm  0.25 lm lm thickness) and
the polar one was a StabilwaxTM consisting of CarbowaxTM-PEG
(60 m  0.2 mm  0.25 mm lm thickness). GCMS spectra were
Fig. 1. Extraction methods of essential oils from citrus fruits (MHG, HD, and CP). obtained using the following conditions: carrier gas He; ow rate
0.3 mL/min; split-less mode; injection volume 1 ll; injection tem-
the extract continuously. Crude juice or extract (in situ water and perature 250 C; the oven temperature programme was 60 C for
metabolites) is collected and separated in receiving asks. It is 8 min increased at 2 C/min to 250 C and held at 250 C for
important to note that this green method allows extracting natural 15 min; the ionisation mode used was electronic impact at 70 eV.
substances without distillation or solvent extraction which are the The relative percentage of the components was calculated from
most energy- and solvent-consuming unit operations. GC-FID peak areas. Most constituents were tentatively identied
N. Bousbia et al. / Journal of Food Engineering 90 (2009) 409413 411

by comparison of their GC Kovats retention indices (RI), deter- 9


Yield (% )
mined with reference to an homologous series of C5C28 n-alkanes
8
and with those of authentic standards available in the authors lab-
oratory. Identication was conrmed when possible by compari- 7
son of their mass spectral fragmentation patterns with those
6
stored in the MS database (National Institute of Standards and
Technology and Wiley libraries) and with mass spectra literature 5
data (de lEurope. Pharmacope Europenne, 1996; Adams, 1995; 4
Arctander, 1994; Recueil des normes franaises, 2000).
3
2.4. Sensory evaluation 2
1
The sensory evaluation of essential oils was conducted by 12 time (min.)
trained panelists who were graduate students and staff members 0
in the laboratory of the University of Avignon. Randomly coded 0 20 40 60 80 100 120 140 160 180 200
samples were individually served to panelists.
Fig. 3. Yield (g EO/g lime peel) prole of lime essential oil obtained by MHG (d) and
HD (s) as function of the extraction time.
2.5. Statistical analysis

The statistical analyses were carried out using the Microsoft ondary metabolites is found in the essential oil isolated by MHG,
Exel software package (Microsoft Corp.) and XLSTAT add-on HD or CP, with relatively similar percentages. Limonene, a mono-
(addinsoft). Canonical discriminant analysis (CDA) was performed terpene hydrocarbon, is the main abundant component in the
with extraction methods (CP, HD and MHG) as dependent variable, essential oil extracted from lime with equivalent relative amounts
concentrations of a-pinene, limonene, b-myrcene, linalool, terpin- for both extraction methods: 70.9%, 71.22% and 71.86%, respec-
4-ol, citronellal, neral, a-terpineol, E-caryophellene, n-nonanal as tively for MHG, HD and CP. Geranial, an oxygenated monoterpene,
explanatory variables. is present at 1.37%, 0.85%, and 1.82%, respectively for MHG, HD and
CP. In this application, microwave irradiation highly accelerated
3. Results and discussion the extraction process, but without causing considerable changes
in the volatile oil composition, a phenomenon which was already
An appropriate microwave irradiation power is important to en- described (Pare and Belanger, 1997; Chen and Spiro, 1995).
sure the essential oil is extracted quickly. However, the power The organoleptic properties of essential oils extracted by MHG,
should not be too high otherwise loss of volatile compounds would HD and CP have been done according to sensory evaluation con-
result. Fig. 2 represents the total extraction time (it was until no ducted by twelve trained panelists who were graduate students
more essential oil was obtained) in relation with the microwave and staff members in the laboratory of the University of Avignon.
irradiation power. A microwave irradiation power of 500 W for Randomly coded samples were individually served to panelists.
500 g of plant material was chosen as an optimum and permits For MHG and CP, the extracted essential oils have the same odour
in only 15 min to extract the essential oil completely. of terpenes hydrocarbons with fresh, light, ora woody and sweet
As shown in Fig. 3, MHG is clearly quicker than conventional citrusy odour. For HD, the essential oil has an odour of terpenes
HD, an extraction time of 15 min with MHG provides yields com- hydrocarbons fresh, pungent but different from fresh fruit and with
parable to those obtained after 180 min by means of HD, which a persistent boiled odour. MHG method offers the possibility for a
is the one of the reference methods in essential oil extraction. better reproduction of natural aroma of the fruit essential oil com-
The overall yield of essential oil obtained from lime peels was parable to CP but more than the hydro-distilled essential oil. MHG
1.0 0.1% and 1.1 0.1% by MHG and HD, respectively. The yield could be a good alternative for the isolation of essential oils from
is expressed as g EO/g citrus fruit. citrus fruits.
The essential oils of lime peels extracted either by MHG, HD or This sensory evaluation has been conrmed by the statistical
CP are rather similar in their composition and contains the same analysis done on 8 varieties of citrus extracted by MHG, HD and
dominant components (Table 1). The same number of volatile sec- CP. Canonical discriminant analysis (CDA) was measured on eight
different citrus fruits considering MHG, HD and CP in order to eval-
uate the inuence of each method on the variety. As shown on
45.00 Fig. 4 and Table 1, extraction procedures are presented on factorial
axis. Canonical discriminant analysis (CDA) was performed with
40.00
extraction methods (CP, HD and MHG) as dependent variable,
Total extraction time (min)

35.00 concentrations of a-pinene, limonene, b-myrcene, linalool, terpin-


30.00 4-ol, citronellal, neral, a-terpineol, E-caryophellene, n-nonanal as
explanatory variables. This graph allows us to conrm that extrac-
25.00
tion procedures are discriminated on factorial axis obtained by
20.00 using initial explained variables. As a consequence, essential oils
15.00 extracted from various citrus fruits with MHG, HD and CP methods
can be easily discriminated, function of the nature of identied
10.00
products but also by their relative proportion. Actually, the 24
5.00 essential oils studied can be classied in 3 distinct subsections rep-
0.00 resenting MHG, HD and CP procedure respectively. It could be eas-
0 200 400 600 800 1000 1200 ily seen that the MHG group is relatively closed to CP group and
Microwave Power (W) different from the HD group. This statistical analysis conrms the
sensory analysis and that essential oil extracted by MHG has an
Fig. 2. Microwave power prole as a function of total extraction time with MHG. odour relatively comparable to CP essential oil.
412 N. Bousbia et al. / Journal of Food Engineering 90 (2009) 409413

Table 1
Chemical compositions of essential oils obtained by SFME, HD, and CP extraction from citrus peels
No. Compoundsa R.I.b R.I.c Eureka Villa Frana Lime Marsh Seedless
MHG HD CP MHG HD CP MHG HD CP MHG HD CP
Monoterpenes 92.10 92.76 93.73 89.68 88.39 93.60 88.70 92.50 95.80 97.93 97.03 97.27
1 Pinene<Alpha-> 926 1023 1.60 1.75 1.62 1.53 1.18 1.02 1.86 1.94 1.62 0.41 0.45 0.27
2 Pinene<Beta-> 974 1109 10.20 15.35 14.00 6.99 7.08 9.24 11.60 13.09 14.00
3 Myrcene<Beta-> 988 1165 1.57 1.33 1.42 1.51 1.52 1.55 1.40 1.46 1.42 1.73 1.81 1.55
4 Carene<Delta-3-> 1101 1290 0.11 0.20 0.15 0.16 0.15 0.15
5 Limonene 1030 1206 69.65 65.25 68.81 70.92 71.22 71.86 60.56 63.44 68.81 95.05 94.21 94.54
6 Terpinene<Gamma-> 1103 1285 8.25 8.08 7.04 7.70 6.58 8.90 11.91 11.17 8.90 0.01 0.03 0.01
Oxygenated Monoterpenes 3.01 3.89 2.65 3.72 3.75 3.65 5.11 4.91 3.71 0.45 0.51 0.36
7 Linalool 1125 1538 0.20 0.18 0.10 0.20 0.35 0.22 0.25 0.36 0.22 0.17 0.18 0.07
8 Citron ellal 1167 1478 0.1 0.05 0.08 0.09 0.06 0.07 0.05 0.05 0.08 0.05 0.02 0.03
9 Terpin-4-ol 1191 1590 0.08 0.42 0.03 0.09 0.37 0.02 0.08 0.19 0.03 0.02 0.09 0.02
10 Terpineol<Alpha-> 1203 1677 0.21 0.56 0.22 0.29 0.53 0.23 0.38 0.37 0.23 0.06 0.08 0.05
11 Nerol 1237 1781 0.26 0.49 0.30 0.44 0.09 0.20 0.13 0.09
12 Neral 1268 1670 0.76 0.68 0.77 0.94 0.53 1.06 1.66 1.55 1.06 0.04 0.03
13 Geraniol 1271 1828 0.24 0.60 0.32 0.56 0.07 0.12 0.07 0.07 0.02 0.02
14 Geranial 1284 1714 1.08 0.89 1.30 1.37 0.85 1.82 2.23 2.05 1.82 0.03 0.04 0.04
Sesquiterpenes 0.85 1.06 1.65 0.99 0.88 2.12 3.56 1.92 1.98 0.49 0.50 1.88
15 Elemene<Beta-> 1373 1583 0.06 0.04 0.08
16 Caryophellene<E-> 1391 1594 0.13 0.18 0.24 0.17 0.16 0.35 0.56 0.31 0.35 0.17 0.20 0.72
17 Bergamotene<Alpha-Trans-> 1437 1577 0.26 0.28 0.50 0.29 0.20 0.58 1.00 0.54 0.58
18 Humulene<Alpha-> 1450 1657 0.03 0.04 0.06 0.03 0.05 0.09 0.13 0.06 0.09 0.04 0.04 0.17
19 Farnesene<(E)-Beta-> 1453 1650 0.01 0.02 0.02 0.01 0.02 0.03 0.06 0.02 0.03
20 Germacrene D 1477 1696 0.05
21 Valencene 1488 1705 0.04 0.01 0.07 0.11
22 Bisabolene<(Z)-Alpha-> 1498 1761 0.02 0.03 0.05 0.03 0.02 0.07 0.10 0.05 0.07
23 Bisabolene(Beta-) 1508 1718 0.38 0.44 0.75 0.43 0.31 0.87 1.51 0.81 0.87
Oxygenated Sesquiterpenes 0.02 0.03 0.03 0.1 0.24 0.04 0.02 0.02 0.03 0.10 0.16 0.26
24 Elemol 1540 1381 0.01 0.01 0.04
25 Nerolidol<E-> 1555 2026 0.01 0.01 0.02
26 Bisabolol<Alpha-> 1684 2212 0.01 0.03 0.03 0.09 0.15 0.04 0.02 0.02 0.03
27 Nootkatone 1799 2250 0.07 0.13 0.15
Other oxygenated compounds 0.95 0.86 0.65 0.75 0.71 0.69 1.19 0.82 0.59 0.52 0.74 0.38
28 Nonanal<N-> 1126 1400 0.08 0.09 0.06 0.10 0.02 0.08 0.04 0.04
29 Citronellyl Acetate 1342 1645 0.02 0.03 0.04 0.02 0.02 0.04 0.04 0.02 0.04 0.01 0.01 0.05
30 Neryl Acetate 1351 1706 0.30 0.26 0.19 0.34 0.36 0.32 0.87 0.60 0.19 0.01 0.01 0.05
Extraction time (min) 15 180 60 15 180 60 15 180 60 15 180 60
Yield (%) 0.7 0.8 0.1 1.6 1.7 0.2 0.8 0.8 0.2 1.0 1.1 0.2
Toal oxygenated compunds (%) 3.98 4.78 3.33 4.57 4.70 4.38 6.32 5.75 4.33 1.07 1.41 1.00
Total non oxygenated compounds (%) 92.95 93.82 95.38 90.57 89.27 95.72 92.26 94.42 97.78 98.42 97.53 99.15

Tarocco Valencia late Washington Naval Tengelo Seminole


MHG HD CP MHG HD CP MHG HD CP MHG HD CP
Monoterpenes 98.02 98.11 98.10 97.57 98.71 98.55 98.33 96.24 98.45 97.48 97.80 97.24
1 Pinene<Alpha-> 926 1023 0.46 0.49 0.50 0.43 0.51 0.52 0.45 0.53 0.50 0.52 0.83 0.91
2 Pinene<Beta-> 974 1109 0.36 0.38 0.37
3 Myrcene<Beta-> 988 1165 1.85 1.87 1.89 1.64 1.85 1.89 1.78 1.76 1.90 1.83 1.79 1.88
4 Carene<Delta-3-> 1101 1290 0.02 0.06 0.01 0.09 0.15 0.20 0.25 0.23 0.28
5 Limonene 1030 1206 95.19 94.68 94.94 94.64 95.48 95.06 95.20 93.16 95.00 90.25 90.34 89.38
6 Terpinene<Gamma-> 1103 1285 0.01 0.05 0.01 0.05 0.06 0.01 3.65 3.78 3.90
Oxygenated Monoterpenes 1.11 0.60 0.61 0.99 0.56 0.64 0.67 0.64 0.29 0.81 1.16 0.57
7 Linalool 1125 1538 0.88 0.17 0.49 0.62 0.30 0.34 0.41 0.27 0.15 0.29 0.62 0.27
8 Citronellal 1167 1478 0.04 0.02 0.02 0.06 0.03 0.05 0.03 0.02 0.04 0.08 0.04 0.08
9 Terpin-4-ol 1191 1590 0.12 0.03 0.06 0.02 0.01 0.12 0.05 0.08 0.01
10 Terpineol<Alpha-> 1203 1677 0.06 0.05 0.04 0.09 0.06 0.05 0.06 0.09 0.02 0.18 0.16 0.10
11 Nerol 1237 1781 0.06
12 Neral 1268 1670 0.05 0.01 0.02 0.05 0.03 0.06 0.07 0.03 0.02 0.01 0.01 0.01
13 Geraniol 1271 1828
14 Geranial 1284 1714 0.05 0.03 0.03 0.09 0.05 0.09 0.07 0.03 0.04
Sesquiterpenes 0.19 0.45 0.26 0.11 0.12 0.13 0.18 0.29 0.38 0.23 0.24 0.35
15 Elemene<Beta-> 1373 1583 0.02 0.01 0.01 0.01 0.02 0.01 0.02 0.02 0.01 0.03 0.04
16 Caryophellene<E-> 1391 1594 0.01 0.01 0.02 0.02 0.01 0.01 0.01 0.01 0.03 0.01 0.01 0.01
17 Bergamotene<Alpha-Trans-> 1437 1577
18 Humulene<Alpha-> 1450 1657 0.01 0.01 0.02 0.03 0.01 0.01
19 Farnesene<(E)-Beta-> 1453 1650 0.01 0.02 0.04
20 Germacrene D 1477 1696 0.01 0.03 0.02 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.02 0.08
21 Valencene 1488 1705 0.12 0.28 0.12 0.02 0.04 0.02 0.13 0.13 0.26 0.15 0.12 0.10
22 Bisabolene<(Z)-Alpha-> 1498 1761
23 Bisabolene(Beta-) 1508 1718
Oxygenated Sesquiterpenes 0.05 0.08 0.02% 0.07% 0.02 0.03 0.02 0.02 0.04 0.05
24 Elemol 1540 1381 0.01 0.01
25 Nerolidol<E-> 1555 2026
26 Bisabolol<Alpha-> 1684 2212
27 Nootkatone 1799 2250 0.01 0.01 0.01 0.01 0.01 0.01
N. Bousbia et al. / Journal of Food Engineering 90 (2009) 409413 413

Table 1 (continued)
Tarocco Valencia late Washington Naval Tengelo Seminole
MHG HD CP MHG HD CP MHG HD CP MHG HD CP
Other oxygenated compounds 0.23 0.24 0.30 0.33 0.26 0.38 0.43 0.31 0.18 0.06 0.07 0.03
28 Nonanal<N-> 1126 1400 0.06 0.02 0.05 0.01 0.03 0.05 0.06 0.04 0.02
29 Citronellyl Acetate 1342 1645 0.01 0.01 0.01
30 Neryl Acetate 1351 1706 0.01 0.01 0.03 0.01

Extraction time (min.) 15 180 60 15 180 60 15 180 60 15 180 60


Yield (%) 1.2 1.3 0.3 1.0 1.1 0.2 0.9 1.0 0.2 1.2 1.3 0.3
Toal oxygenated compunds (%) 1.34 0.89 0.91 1.40 0.84 1.09 1.12 0.98 0.49 0.89 1.26 0.65
Total non oxygenated compounds (%) 98.21 98.56 98.36 97.68 98.83 98.68 98.51 96.53 98.83 97.71 98.04 97.59
a
Essential oil compounds sorted by chemical families and percentages calculated by GC-FID on non-polar HP5MSTM capillary column.
b
Retention indices calculated on non-polar HP5MSTM capillary column.
c
Retention indices calculated on polar CarbowaxTM-PEG capillary column.

4. Conclusion
Observations (axes F1 et F2 : 100.00 %)
3
This is the rst time that microwave heating has been used in
combination with earth gravity to devise a fast and efcient extrac-
2
tion technique. Both the re-design of the glassware and the appli-
cation of microwaves afford a development of a method that serves
F2 (12.47 %)

1 as an example of its usefulness. Microwave hydro-diffusion and


gravity (MHG) makes use of physical and chemical phenomena
0 that are fundamentally different from those applied in conven-
tional solvent extraction and distillation techniques. Using this no-
vel process, fully reproducible extractions can now be completed in
-1
minutes without adding solvent or water. Its additional advantages
are simplied manipulation and work-up, a higher purity of the -
-2 nal product, no need for a post-treatment of waste water and the
consumption of only a fraction of the energy normally required
-3 by conventional food extraction methods.
-5 -4 -3 -2 -1 0 1 2 3
F1 (87.53 %) References

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