ESSENTIAL OILS EXTRACTION METHODS

Parameters affecting the quality

 Seasonal variation
 Geographic variation
 Post harvesting drying and storage of plant tissues
 Method of processing
Pre-extraction preparation of plant samples
 Fresh
 Dry
 Grinded or
 Powdered
1. ENFLEURAGE
Essential Oil Extraction with Cold Fat (Enfleurage)
The principles of enfleurage are simple. Certain flowers (e.g. tuberose and jasmine) continue the
physiological activities of developing and giving off perfume even after picking.
Every jasmine and tuberose flower resembles, a tiny factory continually emitting minute quantities of
perfume. Fat possesses a high power of absorption and, when brought in contact with fragrant flowers,
readily absorbs the perfume emitted.
This principle, methodically applied on a large scale, constitutes enfleurage. During the entire period of
harvest, which lasts for eight to ten weeks, batches of freshly picked flowers are strewn over the surface of
a specially prepared fat base (corps), let there (for 24 h in the case of jasmine and longer in the case of
tuberose), and then replaced by fresh flowers. At the end of the harvest, the fat, which is not renewed during
the process, is saturated with flower oil. Thereafter, the oil is extracted from the fat with alcohol and then
isolated.
Every enfleurage building is equipped with thousands of so called chassis, which serve as vehicles for
holding the fat corps during the process. A chassis consists of a rectangular wooden frame. The frame holds
a glass plate upon both sides of which the fat corps is applied with a spatula at the beginning of the
enfleurage process. When piled one above the other, the chassis form airtight compartments, with a layer
of fat on the upper and lower side of each glass plate.
Every morning during the harvest the freshly picked flowers arrive, and after being cleaned of impurities,
such as leaves and stalks, are strewn by hand on top of the fat layer of each glass plate. Blossoms wet from
dew or rain must never be employed, as any trace of moisture will turn the corps rancid. The chassis are
then piled up and left in the cellars for 24 h or longer, depending upon the type of flowers. The latter rest
in direct contact with one fat layer (the lower one), which acts as a direct solvent whereas the other fat layer
(beneath the glass plate of the (chassis above) absorbs only the volatile perfume given off by the flowers.
Quality & quantity depends on
• Type of fat (soft or hard) (Tallow, Lard)
• Preparation of plant material
2. EXPRESSION:
Cold Pressing
 Odorants are forced out of the natural source by physical pressure
 Fragrant oils obtained using this method is the peels of fruits in the citrus family. This is due to the
large quantity of oil present in the peels of these fruits
 Oil glands in the peel are crushed or broken to release the oil.

Pelatrice Process (pronounced: pel-a-TREE-chay)

1. Citrus fruits are fed from a hopper into the abrasive shell
2. The fruits are rotated against the abrasive shell by a slow-moving screw whose surface rasps the
fruit surfaces causing some of the essential oil cavities on the peel to burst and release their oil-
water emulsion.
3. This screw further transports the fruit into a hopper in which rollers covered with abrasive spikes
burst the remaining oil cavities.
4. The oil and water emulsion is washed away from the fruit by a fine spray of water.
5. The emulsion next passes through a separator where any solids are removed, after which it passes
through two centrifugal separators working in series to yield the pure oil.

Sfumatrice Process (pronounced: SA-fu-ma-TREE-chay)

1. The sfumatrice equipment consists of a metallic chain that is drawn by two horizontal ribbed rollers.
2. The peels are conveyed through these rollers during which time they are pressed and bent to release
their oil.
3. As in pelatrice, the oil is washed away from the sfumatrice rollers by fine sprays of water. Again,
the oil is initially passed through a separator prior to being sent to two centrifuges in series, so that
purified oil can be produced.

3. DISTILLATION

• Common technique for obtaining aromatic compounds from plants

• The raw material (flowers, leaves, wood, bark, roots, seeds, or peel) is heated and the
fragrant compounds are re-collected through condensation of the distilled vapor.
• Distilled products are known either as essential oils or ottos.
Types of Distillation used for Fragrance extraction:

Dry distillation
Hydro distillation
Water distillation
Water and steam distillation
Direct steam distillation

Dry Distillation
1. Direct heating by flame
2. Anhydrous pyrolysis
3. Used for Fossil Amber & Woods, Cade as burned and toasted odor is
desired.

Water Distillation
In this method, the material is completely immersed in water, which is boiled by applying heat by direct
fire, steam jacket, closed steam jacket, closed steam coil or open steam coil. The main characteristic of this
process is that there is direct contact between boiling water and plant material.
Disadvantages of Water Distillation
1. Oil components like esters are sensitive to hydrolysis (since the pH of water is often reduced during
distillation, hydrolytic reactions are facilitated)
RCO-OR' + H2O → RCO-OH + R'-OH
While others like acyclic monoterpene hydrocarbons and aldehydes are susceptible to
polymerization.
 2. Oxygenated components such as phenols have a tendency to dissolve in the still water, so their
complete removal by distillation is not possible.
3. As water distillation tends to be a small operation (operated by one or two persons), it takes a long
time to accumulate much oil, so good quality oil is often mixed with bad quality oil.
4. Water distillation is a slower process than either “water and steam distillation” or “direct steam
distillation”.

Water and Steam Distillation

5. In water and steam distillation, the steam can be generated within the still, although separated from
the plant material.
6. The equipment used is generally similar to that used in water distillation, but the plant material is
supported above the boiling water on a perforated grid.
7. Like water distillation, water and steam distillation is widely used in rural areas. Moreover, it does
not require a great deal more capital expenditure than water distillation. Also, In fact, it is common
that persons performing water distillation eventually progress to water and steam distillation.

Cohobation
Cohobation is a procedure that can only be used during water distillation or water and steam distillation.
It uses the practice of returning the distillate water to the still after the oil has been separated from it so
that it can be re-boiled.
The principal behind it is to minimize the losses of oxygenated components, particularly phenols which
dissolve to some extent in the distillate water.
For most oils, this level of oil loss through solution in water is less than 0.2%, whereas for phenol-rich
oils the amount of oil dissolved in the distillate water is 0.2%-0.7%.
As this material is being constantly re-vaporized, condensed and re-vaporized again, any dissolved
oxygenated constituents will promote hydrolysis and degradation of themselves or other oil
constituents. Similarly, if an oxygenated component is constantly brought in contact with a direct heat
source or side of a still, which is considerably hotter than 100° C, then the chances of degradation are
enhanced.
As a result, the practice of cohobation is not recommended unless the temperature to which
oxygenated constituents in the distillate are exposed is no higher than 100° C.

Direct Steam Distillation

Steam distillation is the most widely accepted process for the production of essential oils on large scale.
Throughout the flavor and fragrance supply business, it is a standard practice.
Direct steam distillation is the process of distilling plant material with steam generated outside the still in a
satellite steam generator generally referred to as a boiler. The plant material is supported on a perforated
grid above the steam inlet.
A real advantage of satellite steam generation is that the amount of steam can be readily controlled.
Because steam is generated in a satellite boiler, the plant material is heated no higher than 100° C and,
consequently, it should not undergo thermal degradation.

Hydro diffusion
Diffusion of essential oils and hot water through plant membranes is known as Hydro diffusion.
When the plant material is soaked with water, exchange of vapors within the tissue is based on their
permeability while in swollen condition. Membranes of plant cells are almost impermeable to volatile oils.
Therefore, in the actual process, at the temperature of boiling water, a part of volatile oil dissolves in the
water present within the glands, and this oil-water solution permeates, by osmosis, the swollen membranes
and finally reaches the outer surface, where the oil is vaporized by passing steam.
Unlike traditional steam distillation, hydro diffusion works off the diffusion principle of allowing steam to
enter the top of the plant charge and diffuse it through the charge by gravity.
The process uses principle of osmotic pressure to diffuse oil from the oil glands. The system is connected
and low pressure steam is passed into the plant material from a boiler from the top.
The condenser, generally of tubular construction which is directly under the basket within the still, is used
for cooling. The oil and water are collected below the condenser in a typical oil separator.
It would appear that hydro diffusion is an efficient process to use as it gives good yield of the oil. But due
to co extraction of other non-volatiles and polar components with the essential oils complicate the process

Solvent Extraction
Maceration
In this process, the whole or coarsely powdered plant is placed in a stoppered container with the solvent
and allowed to stand at room temperature for a period of at least 3 days with frequent agitation until the
soluble matter has dissolved. The mixture then is strained, the marc (the damp solid material) is pressed,
and the combined liquids are clarified by filtration or decantation after standing.
Soxhlet extraction
The process of transferring the partially soluble components of a solid to the liquid phase using a Soxhlet
extractor. The solid is placed in a filter paper thimble which is then placed into the main chamber of the
Soxhlet extractor. The solvent (heated to reflux) travels into the main chamber and the partially soluble
components are slowly transferred to the solvent.
Percolation
Percolation is an extraction process that involves the slow descent of a solvent through a powdered
substance until it absorbs certain constituents and drips out through the filtered bottom of the container.
Problems in Conventional Extraction Methods
1. High temperatures
2. Solvent contamination, reduces product quality
3. Inflammability or explosion risks
4. Time, solvent & energy consuming
5. Composition varies with solvent & extraction technique

Modern (Non-traditional) Methods of Extraction of Essential Oils

Traditional methods of extraction are the methods most widely used on commercial scale. However, with
technological advancement, new techniques have been developed which may not necessarily be widely
used for commercial production of essential oils but are considered valuable in certain situations, such as
the production of costly essential oils in a natural state without any alteration of their thermo sensitive
components or the extraction of essential oils for micro-analysis. Some of these techniques are as follows:
• Supercritical Fluid Extraction (SFE)
• Microwave distillation
• Accelerated Solvent Extraction (ASE)
• Headspace trapping techniques

Supercritical fluid
A supercritical fluid is any substance at a temperature and pressure above its critical point. The supercritical
fluid state occurs when a fluid is above its critical temperature (Tc) and critical pressure (Pc), when it is
between the typical gas and liquid state. At a certain temperature and pressure condition, liquid and vapour
phases of a substance become indistinguishable, known as CRITICAL CONDITION. Substances above
critical point- “SUPERCRITICAL FLUIDS” (SCF)
Manipulating the temperature and pressure of the fluid can solubilize the material of interest and selectively
extract it.
 It can diffuse through solids like a gas, and
 Dissolve materials like a liquid.
 Additionally, close to the critical point, small changes in pressure or temperature result in large
changes in density, allowing many properties of a supercritical fluid to be "fine-tuned".
PROPERTIES OF SCF
• Physical and thermal properties of SCFs are in between pure liquid and gas, hence can also be known as
‘Compressible liquids’ or ‘dense gases’
• Changes in properties are for a SCF are as follows:
– Liquid like densities (100-1000 times greater than gases)
– Diffusivities higher than liquids (10-3 and 10-4cm2/s)
– Good solvating power
– Reduction in surface tension
– Low viscosity (10-100 times less than liquid)
– Gas like compressibility properties
Therefore they possess high penetrating power. Only those having a critical temperature not far from
ambient temperature can be used as alternative solvents for the extraction of essential oils. Carbon
dioxide (CO2), with TC=31.06° C and PC=73.81 bar, is the most attractive solvent, because of its
proprieties regarding toxicity, flammability and cost.

Carbon dioxide and water are the most commonly used supercritical fluids
1. Because it has a near ambient critical temperature (310C), thus biological materials can be
processed at temperatures around 350C.
2. The density of the supercritical CO2 at around 200 bar pressure is close to that of hexane, and the
solvation characteristics are also similar to hexane; thus, it acts as a non-polar solvent.
3. Around the supercritical region, CO2 can dissolve at concentrations up to 1% mass.
4. The major advantage is that a small reduction in temperature, or a slightly larger reduction in
pressure, will result in almost the entire solute precipitating out as the supercritical conditions are
changed or made sub critical.
5. Supercritical fluids can produce a product with no solvent residues.
Advantages
1. Dissolving power of the SCF is controlled by pressure and/or temperature
2. SCF is easily recoverable from the extract due to its volatility
3. Non-toxic solvents leave no harmful residue
4. High boiling components are extracted at relatively low temperatures
5. Separations not possible by more traditional processes can sometimes be effected
6. Thermally labile compounds can be extracted with minimal damage as low temperatures can be
employed by the extraction
Disadvantages
1. Elevated pressure required
2. Compression of solvent requires elaborate recycling measures to reduce energy costs
3. High capital investment for equipment

ACCELARATED SOLVENT EXTRACTION (ASE):

PRINCIPLE OF ASE
EXTRACTION AT VERY HIGH TEMPERATURE AND PRESSURE
• Organic solvents used in extractions boil at relatively low temperatures.
• The highest temperatures at which extractions take place in these techniques will be the
boiling point of the solvent.
• If sufficient pressure is exerted on the solvent during the extractions, solvent temperatures
above the boiling point can be used. This means that all of the advantages of working at
elevated temperature can be realized even with solvents of relatively low boiling points.
• Operating at elevated pressures also helps the extraction process to happen more quickly.
• Pumping solvent through a packed bed is easier at elevated pressures; pressurized solvent
is forced into the pores of the sample matrix.
• Hence, the combination of elevated temperatures and pressures allows extractions to occur
rapidly and completely.
When extractions are achieved at elevated temperatures, several factors contribute to improved
speed, efficiency and reduced solvent use:
1. Solvent strength is higher
2. Diffusion rates are faster due to break of solute–matrix interactions
3. Solvent viscosity is decreased
4. Solute-matrix interactions (dipole attractions, van der Waals forces, hydrogen bonding,
etc.) are more easily disrupted allowing the analytes to be removed from the matrix.
5. The net result means performing extractions at elevated temperatures uses less time and
with less solvent.
PARAMETERS EFFECTING YIELD & QUALITY OF ESSENTIAL OILS

Mode of Distillation;
Technique for the distillation should be chosen on basis of oil boiling point and
nature of herb as the heat content and temperature of steam can alter the
distillation characteristics.

Proper Design of Equipment’s;

Improper designing of tank, condenser or separators can lead to loss of oils and
high capital investments.

Material of Construction of Equipment’s;

Essential oils which are corrosive in nature should be preferably distilled in stills
made of resistant materials like aluminum, copper or stainless steel.

Condition of Raw Material;

Condition of raw material is important because some materials like roots and seeds
will not yield essential oil easily if distilled in their natural state. These materials
have to be crushed, powdered or soaked in water to expose their oil cells.

Filling of Raw Material / Steam Distribution;

Improper loading of the herb may result in steam channeling causing incomplete
distillation.

Operating parameters like Steam Injection Rate, Inlet Pressure/ Condensate
Temperature;
Proper control of injection rates and pressure in boiler operated units is necessary,
to optimize the temperature of extraction for maximal yield
Temperature of condensate should not be high as can result in oil loss due to
evaporation.

Time given for Distillation

Different constituents of the essential oil get distilled in the order of their boiling
points. Thus the highest boiling fractions will be last to come over when, generally,
very little oil is distilling. If the distillation is terminated too soon, the high boiling
constituents will be lost.
TECHNICAL NAMES OF DIFFERENT EXTRACTS

Absolute: Fragrant materials that are purified from a pomade or concrete by soaking
them in ethanol. By using a slightly hydrophilic compound such as ethanol, most of the
fragrant compounds from the waxy source materials can be extracted without dissolving
any of the fragrant waxy molecules. Absolutes are usually found in the form of an oily
liquid.
Concrete: Fragrant materials that have been extracted from raw materials through
solvent extraction using volatile hydrocarbons. Concretes usually contain a large amount
of wax due to the ease in which the solvents dissolve various hydrophobic compounds.
As such concretes are usually further purified through distillation or ethanol based solvent
extraction. Concretes are typically either waxy or resinous solids or thick lily liquids.
Essential oil: Fragrant materials that have been extracted from a source material directly
through distillation or expression and obtained in the form of an oily liquid. Oils extracted
through expression are sometimes called expression oils.
Pomade: A fragrant mass of solid fat created from the enfleurage process in which
odorous compounds in raw materials are absorbed into animal fats. Pomades are found
in the form of an oily and sticky solid.
Tincture: Fragrant materials produced by directly soaking and infusing raw material in
ethanol. Tinctures are typically thin liquids.