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Rosemary oil was extracted by both steam and hydrodistillations then analysed by gas chromatography and gas chromatography–mass spectrometry. The effect of time of extraction enabled us to follow the evolution of the yield and oil composition obtained by both processes. Copyright © 2003 John Wiley & Sons, Ltd.
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Copyright © 2003 John Wiley & Sons, Ltd. Flavour Fragr. J. 2003; 18: 481–484
Flavour Fragr. J. 2003; 18: 481–484
Published online 1 October 2003 in Wiley InterScience ( DOI: 10.1002/ffj.1226
* Correspondence to: C. Boutekedjiret, Ecole Nationale Polytechnique,
Département de Génie Chimique, 10 Avenue Hacene Badi, BP 182, El-
Harrach, Alger, Algérie.
Extraction of rosemary essential oil by steam
distillation and hydrodistillation
C. Boutekedjiret,1 F. Bentahar,2 R. Belabbes1 and J. M. Bessiere3
1Ecole Nationale Polytechnique, Département de Génie Chimique, 10 Avenue Hacene Badi, BP 182, El-Harrach, Alger, Algérie
2Laboratoire des Phénomènes de Transfert, Département de Génie des Procédés, Faculté de Génie Mécanique et Génie des
Procédés, USTHB, BP 32 El Alia, 16111 Bab-Ezzouar, Alger, Algérie
3Ecole Nationale Supérieure de Chimie de Montpellier, 34000 Montpellier, France
Received 5 June 2002
Revised 20 January 2003
Accepted 21 January 2003
ABSTRACT: Rosemary oil was extracted by both steam and hydrodistillations then analysed by gas chromato-
graphy and gas chromatography–mass spectrometry. The effect of time of extraction enabled us to follow the evolu-
tion of the yield and oil composition obtained by both processes. Copyright © 2003 John Wiley & Sons, Ltd.
KEY WORDS: Rosmarinus officinalis L; rosemary; Labiatae; essential oil composition; extraction; steam distilla-
tion; hydrodistillation
Rosemary (Rosmarinus officinalis. L) is an aromatic,
medicinal and condiment plant that belongs to the Family
Labiatae. It is widely spread in Algeria and broadly used
in traditional medicine. Rosemary is selected because it
is of interest as a preservative due to its antioxidative
characteristics and it is used in the pharmaceutical, food
and cosmetic industries. Therefore this work was under-
taken in order to contribute to a better knowledge of the
essences of rosemary coming from the area of Bibans,
located approximately 200 km east of Algiers, and, more
specifically, to compare rosemary essential oils obtained
by steam and hydrodistillations from a qualitative and
quantitative point of view.
The vegetal matter used comes from the ‘Portes de Fer’
in the Bibans area, located 200 km east of Algiers and
identified according to the Flora of Algeria.1 A sample
specimen was deposited in the Herbarium of the Botany
Department at the Algeria National Institute of Agronomy.
Identification of the plant was confirmed by Montpellier
University botanists and the Biology Institute of Algiers
University of Sciences and Technology. Extractions were
realized on a laboratory scale.
To extract the essential oil by steam distillation, the
vegetable matter was placed in a glass column, of which
the lower and higher parts were connected to a water
flask and a condenser, respectively. The water vapour
produced in the flask crosses the plant, charged with
essential oil then to the condenser, where it is condensed.
After condensation, the oil is separated from water by
decantation. The extraction of essential oil by hydro-
distillation was carried out under the same conditions as
the steam distillation. The only difference is that in this
case the vegetable matter is laid out in the flask contain-
ing water and the unit is carried to boiling. The vapour
mixture of water–oil produced in the flask then passes to
the condenser, where it is condensed. The oil is recovered
after decantation.
The essential oils obtained by both extractions
were analysed by gas chromatography (GC) and gas
chromatography–mass spectrometry (GC–MS) under
previously established operating conditions.2,3 A 25 m ×
0.23 mm fused silica capillary column coated with
polydimethylsiloxane (DBP-1) of 1.5 µm film thickness
was the column fitted in the GC an GC–MS systems.
The column temperature was computed to start at 60 °C,
increasing to 200 °C at 3 °C/min. The carrier gas at
1ml/min was nitrogen for GC and helium for GC–MS.
In addition, the oil was recovered at regular time intervals
and analysed by GC in order to follow yield and oil
composition. The essential oil yield was estimated
according to the dry vegetal matter by using the follow-
ing equation:
(%) 100
Copyright © 2003 John Wiley & Sons, Ltd. Flavour Fragr. J. 2003; 18: 481–484
where mHE = essential oil mass (g), mS = dry vegetal
matter mass (g) and RHE = essential oil yield (%).
Results and Discussion
Identification of the Components of the
Essential Oil
The identification of the components of the essential oil
extracted by both steam and hydrodistillations was carried
out by comparison of their mass spectra and retention
times to those of reference standards.4,5 The results are
presented in Table 1.
From this table, it can be seen that these oils were
characterized by the presence of monoterpene hydro-
carbons, oxygenated monoterpenes and sesquiterpenes,
but the quantitative differences were observed in the
contents of these components. The steam distillation
oil composition is comparable to that reported in the
literature,6–13 more specifically to those of the Tunisian
and Greek oils14–15 and to commercial standards.16 This
oil has high monoterpene hydrocarbons and ether con-
tents, even though the water-distilled oil is characterized
by high ketone, alcohol and ester contents. The contents
of the sesquiterpenes were practically the same.
The monoterpene hydrocarbons compounds are in
small proportions in the hydrodistilled oil, due to chem-
ical conversions in the presence of water, resulting from
hydrolysis reactions of these components in monoterpene
alcohol’s components. The quantitative differences in the
rosemary oils composition may be due to extraction pro-
cesses, as previously reported by Boelens.6
Yield and Essential Oil Composition as Function
of Time
The yield of essential oil obtained by the steam distilla-
tion is 1.2%. This value is comparable to that given by
Fournier et al.13 for Tunisian rosemary. The yield of the
hydrodistillation is much lower at only 0.44%. The essen-
tial oil yield as a function of time is shown in Figure 1,
and all oils are recovered after 30 min. In addition, the
yield increases quickly at the beginning of the extraction,
its evolution becoming slower thereafter. Moreover, after
10 min steam distillation more than 80% of essential oil
are recovered; whereas for the hydrodistillation it takes at
least 30 min to extract 88% of the oil.
Analysis by gas chromatography of the oil recovered
with regular time intervals enabled us to follow the
evolution by time of the relative content of some major
components of oil belonging to various known chem-
ical families: 1,8-cineol, camphor, borneol,
bornyl acetate,
-caryophyllene and
-cadinene, as
shown in Figures 2 and 3. Figure 2 shows a rapid evolu-
tion of the content of the considered components, and
those recovered in the ascending order of their boiling
points. Indeed, in the steam distillation, the 1,8-cineol
is mostly recovered in the first 5 min of the process,
followed by camphor, borneol and
-terpineol, which
reach their maximum contents after 10 min extraction;
Table 1. Chemical composition of rosemary essential
oil extracted by steam distillation and hydrodistillation
Components Relative content (%)
Steam distillation Hydrodistillation
-Pinene 5.2 0.4
Camphene 3.0 0.3
-Pinene 5.7 0.3
Myrcene 1.7 tr
-Phellandrene tr tr
p-Cymene 2.2 tr
1,8-Cineol 52.4 31.9
-Terpinene 0.5 tr
Sabinene hydrate 0.3 0.4
Terpinolene 0.2 tr
Linalol 1.1 3.9
Camphor 12.6 19.7
Borneol 3.4 12.1
Terpinene-4-ol 0.7 4.0
-Terpineol 2.1 12.8
Bornyl acetate 1.1 3.1
Thymol tr —
Carvacrol tr —
Eugenol tr —
-Copaene 0.2 0.6
-Caryophyllene 4.2 3.0
-Humulene 0.4 tr
Germacrene D 0.3 tr
-Muurolene 0.2 tr
-Farnesene 0.1 tr
-Cadinene 0.4 tr
Calamenene tr tr
-Cadinene 0.3 tr
Calacorene 0.2 tr
-Cadinene tr tr
Caryophyllene oxide I 0.1 tr
Caryophyllene oxide II 0.1 tr
Humuladienol tr
Humulene oxide tr
Palmitic acid 0.1 tr
Miristic acid tr tr
tr, trace < 0.05%. Figure 1. Evolution of the essential oil yield by time
Copyright © 2003 John Wiley & Sons, Ltd. Flavour Fragr. J. 2003; 18: 481–484
Figure 2. Evolution of the content of some components of rosemary essential oil during steam distillation
The 1,8-cineol and camphor are recovered in greater
proportion after 10 min hydrodistillation, as shown in
Figure 3. We observe thereafter the simultaneous extrac-
tion of borneol,
-terpineol, bornyl acetate and
caryophyllene, which reach their optimal contents after
20 min of the process. After 30 min, only traces of these
components are recovered. In addition, the considered
components are not recovered in the order of their boiling
then the
-caryophyllene follows them with a maximum
content after 15 min and finally the
-cadinene with an
optimal content after 20 min of steam distillation. The
fact that the components considered are recovered in
the ascending order of their boiling points allows us to
suppose that the steam distillation depends on phenomena
of transfer of the oil located at the surface of the plant
and of its evaporation.
Figure 3. Evolution of the content of some components of rosemary essential oil during hydrodistillation
Copyright © 2003 John Wiley & Sons, Ltd. Flavour Fragr. J. 2003; 18: 481–484
points. Indeed, 1,8-cineol is collected at the same time as
camphor, whereas it is more volatile. The same happens
for other components which have different boiling points.
Similar observations were reported by Morin et al.17
for the hydrodistillation of lavender. These authors sug-
gest that the order of exit of the components is dictated
by their polarity and not by their volatility. It is thus
probable that phenomena of diffusion and polarity due to
the action of water intervene simultaneously during the
hydrodistillation of essential oil.
This study made it possible to identify the components of
the essential oils of rosemary obtained by two extraction
processes. Steam distillation seems to be the more suit-
able process, since it gave better yield and an oil com-
position comparable to those reported in the literature and
that recognized by the commercial standards. In addition,
the results obtained show that the duration of extraction
could be limited to 10 min, since more than 80% of oil
is extracted at the end of this time.
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... Currently, hydrodistillation is commonly used for the separation of essential oils from plants. However, these methods often have some problems, such as long reaction times, high energy consumption, and low yields (Boutekedjiret, Bentahar, Belabbes, Bessiere, 2003). Fortunately, some studies have achieved the so-called salting-out effect by adding certain inorganic salts to the system to enhance the distillation process of essential oils (Yang & Zhang, 2017). ...
... Analysis of the essential oil obtained can be done by both GC and GC-MS chromatography methods. In experimental studies, the compounds in the content of the essential oil were detected by comparing the mass spectrometry and retention times of reference standards (Boutekedjiret et al. 2003). ...
Full-text available
Rosmarinus officinalis L. (Rosemary) is a medicinal and aromatic herb belonging to the Lamiaceae family. The geographical distribution of the plant covers especially the Mediterranean Region and regions with a Mediterranean climate. In addition, it has been cultured in many countries around the world so far. The aerial components of the plant, particularly the leaves, are rich in both volatile and nonvolatile phytochemicals: terpenes, flavonoids, phenolic compounds, alcohols, and esters. Phenolic compounds such as carnosol, carnosic acid, and rosmarinic acid in its content have been associated with the plant’s anticancer, anti-inflammatory, antihyperglycemic, antithrombotic, and antioxidant activities. The antimicrobial and antioxidant bioactivities of its essential oil have been utilized and accepted as a safe conservator in the food industry. While the bioactivity of the plant has been proven by in vivo and in vitro experiments, the results of clinical studies support the existence of these bioactivities. The potential of rosemary to be transformed into herbal medicine is considerable. In this chapter, we present an overview of the distribution, ethnobotany, bioactive and nutritional composition and available extraction techniques, scientific evidences, clinical and toxicological studies, available commercial formulations, and challenges and future recommendations as potential drug candidate of rosemary.KeywordsRosemaryPhenolic compoundsRosmarinic acidBiological activity Toxicity
... The combination of hydro-distillation with novel extraction techniques (microwave, ultrasound) have also been reported (Bousbia et al., 2009;. Considering the comparison between steam and hydrodistillation, steam distillation resulted in the extraction of a higher number of compounds in a relatively shorter extraction period of rosemary essential oil (Boutekedjiret, Bentahar, Belabbes, & Bessiere, 2003). ...
Pigments-producing microorganisms are quite common in Nature. However, there is a long journey from the Petri dish to the market place. Twenty-five years ago, scientists wondered if such productions would remain a scientific oddity or become an industrial reality. The answer is not straightforward as processes using fungi, bacteria or yeasts can now indeed provide carotenoids or phycocyanin at an industrial level. Another production factor to consider is peculiar as Monascus red colored food is consumed by more than one billion Asian people; however, still banned in many other countries. European and American consumers will follow as soon as “100%-guaranteed” toxin-free strains (molecular engineered strains, citrinin gene deleted strains) will be developed and commercialized at a world level. For other pigmented biomolecules, some laboratories and companies invested and continue to invest a lot of money as any combination of new source and/or new pigment requires a lot of experimental work, process optimization, toxicological studies, and regulatory approval. Time will tell whether investments in pigments such as azaphilones or anthraquinones were justified. Future trends involve combinatorial engineering, gene knock-out, and the production of niche pigments not found in plants such as C50 carotenoids or aryl carotenoids.
... Năm 2003, C. Boutekedjiret cùng cộng sự đã so sánh hiệu quả chưng cất tinh dầu Hương thảo bằng phương pháp chưng cất trực tiếp và chưng cất hơi nước. Kết quả cho thấy, chưng cất hơi nước cho hiệu suất cao hơn chưng cất trực tiếp là 0,44% [6]. Năm 2008, N. Bousbia cùng cộng sự đã so sánh phương pháp chưng cất trực tiếp và chưng cất có sự hỗ trợ của vi sóng. ...
Cây Hương thảo du nhập vào Việt Nam khoảng năm 2007. Tinh dầu Hương thảo có các đặc tính chống oxi hóa, kháng khuẩn, kháng nấm; được chiết xuất bằng các phương pháp: chưng cất trực tiếp trong nước, chưng cất hơi nước, chưng cất trực tiếp có sự hỗ trợ của vi sóng hoặc sóng siêu âm. Bài báo nghiên cứu các yếu tố ảnh hưởng đến quá trình chưng cất hơi nước. Hiệu suất tinh dầu thu được là 3,04% với các điều kiện: 300g nhập liệu Hương thảo khô xay (0,1-0,3cm), nhiệt độ nồi đun 1950C trong 70 phút (cho tốc độ bay hơi 0,045ml/s). Kết quả phân tích bằng GC-MS cho thấy các thành phần chính có trong tinh dầu: α-pinene 23,63%, 1,8-cineole 15,349%, borneol 5,563% và geraniol 5,517%. Thực hiện so sánh hiệu suất và thành phần tinh dầu thu được với các phương pháp chưng cất trực tiếp trong nước và chưng cất có sự hỗ trợ của vi sóng.
... The variation of supercritical fluids thermodynamic properties influences, mass transfer between the solute to extract and the CO 2 and, consequently, in the selectivity of the target compounds (Chemat et al., 2017). Concerning the extracts composition (Table 1) borneol and α-pinene as the main compounds provided from R. officinalis herb extracted by SFE-CO 2 (Ibáñez et al., 1999) and hydrodistillation processes (Boutekedjiret et al., 2003;Elyemni et al., 2019;Jamshidi et al., 2009;Mena et al., 2016). Thus, despite the effect of the extraction method, pre-treatment, nature and environmental conditions of the plant material production, similar chemical composition was found. ...
... Plants were dried by shadow drying method for 6-8 days and then grinded. Essential oils were obtained by steam distillation as previously described [14,15]. The collected EO was stored in amber color bottles at room temperature until use. ...
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We have investigated the antibacterial, anti-biofilm, and anti-quorum sensing potencies of six Essential Oils (EOs) obtained from cinnamon (Cinnamomum verum), thyme (Thymus vulgaris), clove (Eugenia caryophyllata), curcuma (Curcuma longa L.), rosemary (Rosmarinus officinalis L.), and sage (Salvia officinalis). The study was conducted on 20 multidrug-resistant (MDR) S. enteritidis clinical strains. Minimum inhibitory concentrations and minimum bactericide concentrations were displayed by microdilution. The effect on biofilm formation was tested on polystyrene plates. The anti-quorum sensing effect was determined by measuring the inhibition of violacein production by Chromobacterium violaceum CV026. The influence of EOs on the adhesion of Salmonella strains to HT-29 cells was studied. The potency of S. enteritidis to infect and kill Caenorhabditis elegans was evaluated. The cinnamon, thyme, and clove EOs showed remarkable antibacterial properties. Biofilm formation was significantly reduced by the six EOs: 99.10% for cinnamon, 97.64% for clove, 95.90% for thyme, 79.84% for rosemary, 28.98% for curcuma, and 15.55% for sage. The MIC/2 of clove EO exhibited the highest percentage of inhibition of violacein production (99.03%), followed by thyme (91.68%) and cinnamon (84.13%) EOs. Thyme extracts exhibited an important anti-adhesive potency. Clove EO behaves as an effective regulator of Salmonella virulence in nematodes.
An improved method denoted as salting out-solvent-free microwave rotary distillation (SOSFMRD) was successfully developed for the extraction of essential oils from fresh magnolia (Oyama sieboldii) leaves, in which we achieved the rotation of the reaction material by means of a rotating motor to subject the material to uniform microwave irradiation. Magnesium chloride was selected as the salting-out agent through a comparative study on the salting-out effects of different anions and cations of metal salts. The variables of SOSFMRD were systematically optimized. Under the obtained optimization conditions, the essential oil yield was 21.68 ± 1.02 mL/kgDW. Gas chromatography–mass spectrometry analysis showed that the main chemical constituent of O. sieboldii essential oil was dehydrocostuslactone, the content of which reached 30.23 ± 1.27%. Compared with the other conventional methods, this method has a high yield and low energy consumption, which can effectively reduce impact on the environment.
Essential oils have many interesting applications in industry food, cosmetics, pharmaceutical, agriculture. Essential oils can be produced by various techniques, including conventional, novel and biotechnology methods. Novel extraction methods can be considered as a good alternative to conventional methods due to short extraction time, high efficiency and quality, non-decomposition of compounds due to heat and no pollution. Recently, due to the limitations of extraction methods, the attention of scientists has been focused on synthesizing aromatic compounds through biotechnological methods. In the biotechnology method, there is no concern about factors such as climate conditions, supply shortages, natural disasters, plant disease and a high-quality product is obtained. Biotechnology could provide an environmentally friendly alternative that does not require as much land and resources as traditional methods. This review covers up-to-date literature on extraction methods of essential oils, including conventional methods, novel methods and biotech methods, and a generally comparison between them.
To overcome the problem of organic waste originating from citrus peels, research on essential oils from various species of citrus peels is necessary. This study was performed to determine chemical components in citrus peel essential oils from four species: Citrus sinensis (L.) Osbeck (sweet orange), Citrus reticulata Blanco (tangerine), Citrus aurantifolia (Christm.) Swingle (lime), and Citrus limon (L.) Burm.f. (lemon) growing in Indonesia, including their respective antibacterial and antioxidant activities. The chemical components were identified with GC/MS analysis, the antioxidant activity was tested using DPPH method, and antibacterial activity was determined by Paper Disc Diffusion method. Tangerine, sweet orange, lemon, and lime peels essential oils were source of d-limonene, with levels of 83.95%, 83.00%, 49.41% and 21.27%, respectively. Five same chemical components identified in all citrus peels essential oils were d-limonene, α-pinene, sabinene, β-myrcene, and linalool. The order of antibacterial activity against Staphylococcus aureus ATCC 6538 from the strongest were lime (very strong), followed by lemon (strong), sweet orange (strong), and tangerine (moderate) peels essential oils. The order of antibacterial activity against Escherichia coli ATCC 11229 was lime (strong), followed by tangerine (moderate), lemon (moderate), and sweet orange (moderate) peels essential oils. All of the citrus peels essential oils in this study had strong antioxidant activity. These findings indicated that sweet orange, tangerine, lime, and lemon peels essential oils could be an excellent source of d-limonene, natural antioxidants and antibacterial agents, which might be utilized in cosmetics, foods, or pharmaceuticals industries and further studies are warranted.
An infection by pathogenic fungi is one of the major problem in post-harvest stage of mangoes. Therefore, the extraction of essential oil from Melaleuca alternifolia is being tested as a natural fungicide for controlling fungus infections of selected mangoes locally known as susu mango. The extraction was performed using Solvent-Free Microwave Assisted Extraction with a yield of 0.57% concentration. The inhibitory effect of this essential oil against isolated fungi from mango was investigated through in-vitro and in-vivo analyses. Distilled water was used as a negative control while chemical fungicide (Globus 5.5) was used as a positive control in the analyses. The mycelial growth inhibition of the extracted essential oil for poisoned food test and disc diffusion method showed 62.50 ± 0.49% and 59.70 ± 0.30% respectively for in-vivo experiment which used unwounded and artificially wounded mangoes. The result also demonstrated that the essential oil applied on the mangoes could decrease the disease incidence from 100% to 61.33% for up to 10 days incubation at room temperature compared to that of the control. Hence, the essential oil of Melaleuca alternifolia can act as a green fungicide and is also a promising alternative to the synthetic chemical fungicide for controlling post-harvest disease on mangoes.
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The essential oil of Rosmarinus officinalis L. from Algeria was analyzed by GC and GC/MS. More than 90% of the components were identified with 1,8-cineole (52.4%) and camphor (12.6%) being the major components.
The essential oils of Rosmarinus eriocalyx which were produced from the leaves of six populations of plants collected in Algeria under different ecological conditions were analysed by GC and GC/MS. In R. eriocalyx 36 compounds were identified, with camphor (32.3–37.0%), camphene (17.0–20.0%), a-pinene (15.2–18.2%) and 1,8-cineole (7.6–11.4%) as main components in all samples. In order to permit comparison, analyses were also conducted on the essential oil of R. officinalis from Spain and Italy. Also in this case the principal component was camphor (35.3% and 17.7%), followed by 1,8-cineole (24.0% and 23.5%) and limonene (11.0% and 9.5%). It has been demonstrated that quantitative differences in α-pinene, β-pinene, 1,8-cineole and camphor exist when our results are compared with these previously published.
Because of its sensitivity to cold, rosemary was not previously cultivated in Hungary. As a result of the selection work, we have been successful in isolating a frost-resistant selection of rosemary, the cultivation of which is now underway. The composition of the oil of this new rosemary selection is slightly different to other rosemary oils. The major components of the oil were α-pinene (4.1–14.4%), 3-octanone (trace-10.0%), β-pinene (5.3–13.7%), 1,8-cineole (21.3–46.4%), camphor (13.0–31.0%) and verbenone (2.5–11.1%). Among the components identified by GC and GC/MS, 3-octanone and verbenone were found to be the characteristic constituents of the oil of the new Hungarian selection. It was also found to possess antimicrobial activity.
Etudes de divers échantillons d'huiles essentielles de Romarin de Tunisie
  • G Fournier
  • J Habib
  • A Reguigui
Fournier G, Habib J, Reguigui A et al. Etudes de divers échantillons d'huiles essentielles de Romarin de Tunisie. Plant. Médicin. Phytothé., 1983; 23(3): 180-185.