To optimize this domestic process, a 2 Principal component analysis of samples obtained with the experimental design, and their radar plots, indicated a very strong resemblance between oils obtained from the same plant part, and a marked difference between those obtained from different plant parts.
International
Journal of Engineering Science Technologies, 2(1), 37-57. doi: 10.29121/IJOEST.v2.i1.2017.05
The
genus
In the
first description we published in 2006 of the essential oils from different
parts of the plant (roots, stems, leaves, flowers), we reported that the oils
from the aerial parts were mainly composed of In a
previous very detailed study of (i) the
volatile components from stems and roots obtained by hydrodistillation and
head-space SPME, and (ii) the phenolic compounds and flavonoids extracted with
methanol, ethyl acetate and dichloromethane, the antioxidant activities of the
extracts were demonstrated and compared [8]. Loumouamou
However,
the massive presence of Further,
aristolone, a ketone that is very abundant in the roots, could either be
isolated or gainfully used in its native state, or after conversion into its
oxime: several studies have found this family of substances to have antitumor,
antimicrobial, antioxidant, and antidepressant, anticonvulsive and antiviral
properties [18]. We
describe here the essential oil extraction from stems and roots of The
results of this work will support controlled artisanal production of this oil,
which is of potential medicinal interest, by essential oil producers grouped in
the OIBT project as part of the Republic of Congo anti-poverty programme [19].
In the
Republic of Congo, where it grows under the lower-Congo climate, on clay-sand
to sandy-moist soil, this plant, which does not exceed 1 m in height,
presents upwardly branched culms, thin sinuous roots 4–8 cm long, rolled leaves
8–15 cm long and 2 cm wide, and a glabrous base.
Figure 1: Fresh
Plant of Elyonurus Hensii (Stems, Leaves, Flowers, Roots,) The
samples studied were collected on the “Plateau des Cataractes” at Loufoulakari,
Loukoko and Sese (District of Louingui, Pool Department, R Congo).
In the Laboratory scale, the essential oils were obtained by steam distillation. Water and plant material (200 g of plant material for stems, or 135 g for roots.) were placed in a Clevenger apparatus for 4 h. The organic phase of the resulting condensate was separated from the aqueous phase by extraction with diethyl ether. The organic phase was dried over sodium sulphate and the essential oil was recovered after evaporation of the solvent. The artisanal extraction is led in a cylindrical distiller (60 L, 4kg). The vapor resulting from the hydrodistllation passes in a pipe (2 cm diameter) crossing a (100 cm length, 30 cm broad and 30 cm height) reserve, filled with cool water circulating in opposite direction (figure 2).
Figure 2: Local equipment for hydrodistillation of essential oils (60 L)
GC analysis was performed on an Agilent GC 6890
instrument equiped with a split injector
(280°C), a flam ionization detector (FID) and a DB-5 column (20m x 0,18mm x
0,18µm).The temperature program was 50°C (3.2 min) rising to 330°C (10°C /min). Dihydrogene was used as
carrier at a flow rate 1ml/min.
GC/SM analysis was performed on Agilent GC 7890 /Agilent MS 5975 operating in EI mode (70 eV), equiped with a DB-5 column (20m x 0,18mm x 0, 18µm). The temperature of injector was 280°C and helium was the carrier gas at 0.9 mL/min. The temperature program was 50°C (3.2 min) rising to 330°C (8°C /min). The identification was carried out by calculating retention indices (RI) and comparing mass spectra with those in data bancks [22], [23], [24], [25].
The
variables influencing extraction yield were:
time, temperature, condensation rate, the state of division of the plant
material, the mass ratio of plant material to water, and water loss from
plant material [26]. A model
with six variables, even in the case of a first degree model, would need 2 The
experiment is designed to determine the effects of certain factors on each
response. The
two-level factorial design as developed by Davies [28] is well-suited to
addressing this type of question, and has the advantage of needing only very
elementary mathematical skills [29].The
general formula for a complete factorial plan with N experiments is N = 2 To
construct the experiment matrix we define reduced variables x x Table 1: Levels of the variables in steam extraction of Elionurus
The combination of these 3 variables and the 2 levels by variable lead to the following experimental design (table 2) Table 2: Experimental design for essential oil extraction from Elionurus hensii stems
The domain of the study, with coded variables, becomes the domain (-1, +1) and the eight responses described by the experimental matrix are set up after randomisation (table 3). Table 3: Experimental matrix for essential oil
extraction from Elionurus hensii stems
For a
first degree model with interactions, the representative points of a
three-variable experimental design are located in three-dimensional space. The
corresponding response function is a first degree polynomial for each factor
taken separately. It is notated: y = a
If the
mathematical model associated with the factorial design is constructed with
centred, reduced variables, the coefficients of the polynomial thus have very
simple meanings: average a, and _{ij}a[27]._{ijk }
Means, standard deviations and the usual graphs were obtained with Excel software. Multivariate analysis was performed on XLSTAT software (Addinsoft an add up of Excel Microsoft).
Previously
works show that the essential oils from all the aerial
parts were similar, and were mostly composed of oxygenated monoterpenes, in
particular Tables 4
and 5 show respectively chemical composition of stem and root essential oils
from Table 4: Chemical composition of the essential
oil from stems of Elionurus hensii (Loufoulakari site)
Table 5: Chemical composition on root essential oil (Loufoulakari
site)
Table 6: Major constituents (**)
of essential oils from stems (S) and roots (R) collected at the sites of
Loufoulakari (sample 1), Loukoko (sample 2), and Sese (sample 3)
* S1 means: stem of
sample 1; R2: root of sample 2) The
essential oil from stems was composed of a large number of menthadienol isomers
like in These
oils differed appreciably from those extracted from roots, which had lower
essential oil contents, more Aristolone
was isolated and identified spectrally by NMR spectroscopy and mass
spectrometry [10] This difference
can be visualised using a polar coordinate representation (radar plot). One
notes that (i) the radar plot of the essential oil from stems differs from that
of oil from roots, and (ii) those of oils from the same parts of the plant
(stems or roots) are similar. Figure 3 shows radar plots of stem and root
essential oils. Figure 3:
Radar- plots of Stem and root essential oilsextracted from
Steam
distillation and water distillation are used to extract useful essential oils from
aromatic plant resources. Skaria Only hydro-distillation and vapo-hydro-distillation can be used at artisanal scale.
The
modelling of the extraction process is in principle complex, but can be
simplified by a judicious choice of the factors to be studied. We selected
three factors: extraction duration (h),
X Table 7
recapitulates the experimental matrix and the responses: essential oil content
and cumulated Table 7: Experimental matrix and responses (essential oil
content and cumulated
The mathematical equation
representing the quantitative yield of the hydrodistillation of stems of
x_{3 }+ 0.04x_{1}x_{2} – 0.001x_{1}x_{3} – 0.17x_{2}x_{3}_{ }+
0.10x_{1}x_{2}x_{3}_{}With:
This
relation shows that the optimum should be located in the experimental domain or
very close to it, as the values of The
influence of residual water content
( The mathematical equation
representing the cumulated
_{
}– 0.563x_{3} + 1.578x + 0.658x_{1}x_{2}_{1}x_{3}
+ 0.128x_{2}x_{3} + 0.366x_{1}x_{2}x_{3}The
average content of cumulated
Tables 8
and 9 give the levels of variation of the three variables, the experimental
matrix, and the responses (essential oil yield and aristolone content). Table 8. Levels of variation of variables
forthe extraction of essential oils from Elionurus hensii (roots)
Table 9: Experimental matrix and responses forthe
extraction of essential oils from Elionurus hensii (roots)
The mathematical equation
representing the quantitative yield of the hydrodistillation of roots of y = _{2} + 0.0575x_{3} – 0.0725x_{1}x_{2 }–
0.0375x_{2}x_{3} + 0.0775x_{1}x_{3} + 0.0975x_{1}x_{2}x_{3}Average yield
(0.747), effects of factors (0.0575 - 0.112) and effects of interactions (0.0375 –
0.0775) are less important in root essential oil extraction. The extraction duration
presents the most important positive effect. Interaction effects are negligeted. The mathematical equation
representing the aristolone content in essential oils of
Aristolone
extraction is more sensitive to the effects of factors and interactions. With an
average yield of 41.181 %, the extraction was impacted by the residual water
content (3.466) and the interaction of extraction duration/state of division
(3.516).The three- factor interaction lead to the most important effect on the
response (4.133).
The analysis
of essential oils collected during the execution of the experimental
design can yield information on how the
different constituents of these oils are extracted in relation to the factors
studied. If light
fractions are collected first during a distillation, we can expect to obtain
oils rich in light fractions for short times and rich in heavy fractions for
long times. If by
contrast all the constituents are collected at the steam temperature, the parts
affected first by the steam will be collected together, and we can expect an
oil that from the very first drop will have the average composition of the
plant’s total essential oil. The
multivariate analysis of 16 samples from two experimental designs gave very
interesting results. Principal
component analysis (PCA) carried out on the data given in Tables 11 and 12
indicates a very close correlation of variables, mainly around the first
principal axis (F1) in the first principal plane (F1F2). Table 10: Yield (%) and major
component contents (Table 6 *) in
essential oils from stems (S**) and roots (R***) of Elionurus hensii obtained in
the execution of the experimental design
This means
that the analysis can be carried out with a much smaller number of variables
(constituents of essential oils). Ten of the 16 variables used lie on the
correlation circle. F1 contains
75,25 % of the information on the variability of the essential oils, and 83,14
% on F1F2. The study can therefore be limited to the first principal plane F1F2
(Figure 4). Figure 4: Correlation circle of variables in principal component
analysis (PCA) The
distribution of individuals in the first principal plane F1F2 shows a clear
separation between oils of the plant’s aerial parts and those of its
below-ground parts, suggesting a close similarity of oils from the same plant
part, and a marked difference in the oils from the two parts (Figure 5). Figure 5: Distribution of individuals (essential oil samples) in principal
component analysis (R: roots; S: stems) Ascending
Hierarchical Clustering (AHC) confirms the distribution into two groups each
totally separate and homogeneous (oils from stems and oils from roots)
(Figure 6, Table 11). Figure 6: Classes generated by
HAC of essential oils Table 11: Distribution of
individuals into classes by HAC
A local extractor, used in a domestic scale in Table 12: Levels of variation of variables in the artisanal extraction of essential oils from Elionurus hensii (aerial parts).
Table 13: Experimental matrix and responses for the extraction
of essential oils from
The average of yield of essential oil extraction is 0.75. Figure 7 gives the values and the relative importance of the principal and interaction effects of the first order factor. The principal effects b The mathematical expression of the first degree polynom associated to the full factorial design model selected here is: y = 0.75 + 0.03 x
With a coefficient of regression R
Figure 7: Graphic representation of the coefficient of factor effects (principal and interaction) on the yield of essential oil extraction. Figure
8: Graphic representation of factor interaction effectson the yield of essential oil extraction.
The statistics of the coefficients of the model leading
to the coefficient of regression R z= 40.0 -0.055x The average of the
Figure 9: Graphic representation of the coefficient of factor effects (principal
and interaction) on
The composition of 8 samples extracted Table 14: Essential oil composition of samples extracted via the artisanal experimental design (Elionurus hensii stems).
Figure 10: Representative radar plot of the essential oil
extracted
Hydrodistillation
is used to extract useful essential oils from aromatic plant resources. Their efficiency depends on both the plant
material and the extraction process. It
is important to work with homogeneous plant material obtained in the most
favourable conditions (collection of plant material when the content and
composition of the essential oil is optimal) The
modelling of the extraction process is in principle complex, but can be
simplified by a judicious choice of the factors to be studied. We selected
three factors for the steam distillation and four factors for the water
distillation. These were used as variables in a two-level factorial design.
This design, involving a mathematical model in the form of a first degree
polynomial, was used to calculate average response, and effects of factors. The factor considered and the experimental domain selected have very weak influence on the extraction of the essential oil, which is on average 0, 75 %. For the aerial part (stems, leaves and flowers) of The effects of these same factors have impact more
important on the contents of The composition of the 8 samples resulting from the experimental design have a similar compositions; the factor studied do not have any impact on the quality of oils: nearly 50 % of p-menthadienols, which are responsible known biological properties of this plant.
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