EXTRACTION

Guided by Prepared by
Dr.A.U.Tatiya Mr.Vishal S Bagul
M.Pharm 1st Sem. (2015-20146
Department of Pharmacognosy
R.C.Patel Institute of Pharmaceutical
Education and Research, Shirpur.
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 Extraction:
 Extraction is the method of removing active constituents from a
solid or liquid by means of liquid solvent.
 The separation of medicinally active portions of plant or animal
tissues from the inactive or inert components by using selective
solvents.
 In this method the wanted components are dissolved by the use of
selective solvents known as menstrum & undissolved part is a marc.
After the extraction unwanted matter is removed.
Extracts are prepared by using ethanol or other suitable solvent.
 Extract : Extracts can be defined as preparations of crude drugs
which contain all the constituents which are soluble in the solvent.

Marc: Solid residue obtain after extraction

Menstruum: Solvent
S used for extraction
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  Type of extracts
◦ Dry extract (Tab, cap.)
E.g. belladonna extract
◦ Soft (Ointment, suppository)
E.g. glycerrhiza extract.
◦ Liquid : As tincture.

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 Dissolution of extractive substances out of
disintegrated cells.
 Dissolution of extractive substances out of intact
plant cell by diffusion (requires steeping and
swelling)
 Penetration of the solvent into
the plant cells and swelling of
the cells.
 Diffusion of the dissolved
extractive substances out of the
cell.

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 Plant constituents are usually contained inside the
cells. Therefore, The solvent used for extraction must
diffuse into the cell to dissolve the desired compounds
whereupon the solution must pass the cell wall in the
opposite direction and mix with the surrounding liquid
.
An equilibrium is established between the solute
inside the cells and the solvent surrounding the
fragmented plant tissues

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 Ideal properties of the solvents :
1. Be highly selective for the compound to be extracted.
2. Not react with the extracted compound or with other
compounds in the plant material
3. Have a low price.
4. Be harmless to man and to the environment.
5. Be completely volatile.
6. Should not mix up with water.
7. Should have the big capacity in relation to extractive.
8. The density of solvent should be difference from water
density.
9. Should have the minimum viscosity.

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Mechanism of Extraction :

solvent

Plant 2
cell

7 3
Factors affecting extraction process :
Nature of drug
Solvent
Temperature
pH
Particle size

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 Methods of extraction :
 Infusion
 Decoction
 Digestion
 Maceration
 Percolation
 Continues hot extraction
 Supercritical fluid extraction
 Counter current extraction
 Microwave assisted extraction
 Ultrasonication-Assisted Extraction:

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Infusion :
Fresh infusions are prepared
by macerating the crude drug
for a short period of time with
cold or boiling water. These are
dilute solutions of the readily
soluble constituents of crude drugs.
Types of Infusion :
 Fresh Infusion : e.g. Infusion of orange
 Concentrated Infusion : e.g. Concentrated
infusion of Quassia

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Decoction :
In this process, the crude
drug is boiled in a specified
volume of water for a defined
time; it is then cooled and
strained or filtered. This
procedure is suitable for
extracting water-soluble,
heat stable constituents.
e.g. Tea , Coffee

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 Digestion :
 This is a form of maceration in
which gentle heat is used during
the process of extraction.
 It is used when moderately
elevated temperature is not
objectionable. The solvent
efficiency of the menstruum is
thereby increased.
e.g. Extraction of Morphine

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 Maceration :
In this process solid ingredients
are placed in a stoppered container
with the whole of the solvent and
allowed to stand for a period of at
least 3 days (3 - 7 days) with frequent
agitation, until soluble matter is
dissolved. The mixture is then strained
(through sieves / nets), the marc pressed
and the combined liquids clarified
(cleaned by filtration) or by decantation, after standing.

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 Process of maceration :
Flow chart
Plant Material
(Crushed or cut small or Placed in a closed vessels
Moderately coarse powder)

Whole of the selected solvent

Allowed to stand for seven days
(Menstruum)added
shaking occasionally

Solid residue (marc)

Liquid strained off pressed(Recover as much as
occluded solution)

Clarified by subsidence or (Strained and expressed

filtration liquids mixed)

14 Evaporation and Concentration

 Types of maceration :
 Simple maceration: for organized and unorganized Crude drug
e.g. i) Tincture of Orange
ii) Tincture of Lemon
iii) Tincture of Squill
 Double maceration : Concentrated infusion of orange
 Triple maceration: The maceration process may
be carried out with help of heat or stirring
e.g. i) Concentrated infusion of Quassia
ii) Concentrated infusion of Senna

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 SIMPLE MACERATION:-

INTRODUCTION:-
The extraction of the drug with a solvent with
several daily shakings or stirrings at room
temperature.
In this type of maceration, organized drug are used.
TYPES:-
1.Kinetic maceration: is carried out at room
temperature, like simple maceration, the difference
being that the material is kept in constant motion.
2.Vortical (turbo) Extraction:-The drug is stirred in the menstrum
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with a high-speed mixture or homogenizer
 THEORY:-
The extraction of the drug with a solvent with several
daily shakings or stirrings at room temperature.
Where,
weight of solute diffusing = W
Diffusion coefficient = D
Surface area = A
Concentration of solute at
interface=C1
Concentration of solute in bulk =
C2
DA (C1-C2) θ Thickness of boundary layer = L
W = --------------------- Time = θ
17 L
 THEORIES OF MACERATION:-
Schoenemann’s Diffusion theory

The rate of extraction depends on the rate of diffusion

Boucher et al., Soaking theory

Not only the rate of diffusion but also the rate of dissolution of the substances in
the solvent critically affect the rate of extraction

Karnowsky’s Capillary velocity Theory

It represents the rate of extraction as a function of the rate of flow in the

capillaries.

Schultz & Koltz theory of maceration

C = amq

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 Factors affecting Maceration
Concentration gradient (C1-C2) is affected by several factors
1.Solid/solvent ratio: Yield decreases with constant quantity of solvent and
increasing proportion of drug material.
2.Dissolution from disintegrated cells: Particle size
3.Steeping and swelling of plant material: Capillary dilation and increase in
diffusion rate (Mucilage)
4.Diffusion from intact plant cell: Solvent must be able to solublilize
substances
5.Temperature: increase solubility (diffusion coefficient), and decrease the
viscosity
6.pH value: Influence the selectivity of extraction (qualitative and quantitative)
7.Interaction of dissolved constituents with insoluble support material of plant
8.Degree of lipophilicity
19 9.Effect of addition of surfactants, salts and co-solvents
 MODIFIED MACERATION:-

INTRODUCTION:-
In this type of maceration unorganized drug are used
which have no cellular or tissue structure.
eg. Gum, Resins, Gum-resins, Oleo gum-resins.
Here, unorganized drugs are used because in short time
complete reaction not takes place. Because of no cellular
structure in unorganized drugs, soluble components are
directly exposed to menstrum so the process is quicker.
Here the whole procedure is like simple maceration but
the final product is not collected by pressing the marc but
it is adjusted to the definite volume.

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 MULTIPLE MACERATION-

The aim of multiple maceration is to achieve maximum

extraction by using proteins of the total volume of menstrum
for successive maceration.
The volume of menstrum calculated as follows:-
VACUUM MACERATION:-

It employs a designed maceration vessel with arrangement

for connecting it to vacuum line.
Modification increase its permeability of cell walls
considerably & facilitates extraction in much shorter time

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 Merits
 Small sample size.
 Strong swelling properties or high mucilage.
 Energy saving process.

Demerits
 Not exhaustively extract the drug.
 It is very slow process.
 Solvent required is more.

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Percolation :
 It is continuous downward displacement
of the solvent through the bed of crude
drug material to get extract.

 Most frequently used to extract

active ingredients in the preparation
of tinctures and fluid extracts.

 It is the method of short successive

maceration or process of displacement

 A percolator (a narrow, cone-shaped

vessel open at both ends) is conical cylindrical
generally used.
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Steps in percolation :
 1. Size reduction: The drug to be extracted is subjected to suitable
degree of size reduction, usually from coarse powder to fine
powder.
 2. Imbibition: During imbibition the powdered drug is moistened
with a suitable amount of menstruum and allowed to stand for four
hours in a well closed container.
 3. Packing: After imbibition the moistened drug is evenly packed
into the percolator.
 4. Maceration: After packing sufficient menstruum is added to
saturate the material. The percolator is allowed to stand for 24 hours
to macerate the drug.
 5. Percolation: The lower tap is opened and liquid collected therein
is allowed to drip slowly at a controlled rate until 3/4th volume of
the finished product is obtained.

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 Types of Percolation :
1.Simple Percolation :
Drug Percolation and collect
Imbibition Maceration the percolate i.e.3/4th
200gms For 4 hours For 24 hours of the volume of
e.g. i) Tincture of Belladonna finished preparation
ii) Compound tincture of cardamom

2. Modified Percolation :
 Repeated maceration is more effective than simple.
 Multiple maceration – Solvent divided into equal multiple time
considering the solvent retained by plant tissue.
 Used to prepare concentrated preparation.
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 Reserved percolation:

 In this case the extraction is done through the general

percolation procedure.

 At the last, the evaporation is done under reduced pressure

in equipment like a Climbing evaporator to the consistency
of a soft extract (semi solid) such that all the water is
removed.

 This is then dissolved in the reserved portion which is

strongly alcoholic and easily dissolves the evaporated
portion with any risk of precipitation.

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 Merits :
Requires less time than maceration.
Extraction of thermolabile constituents can be possible.

Demerits :
Requires more time than soxhalation.
More solvent is required.
Skilled person is required.

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 Maceration Vs Percolation

Maceration Percolation
• Time consuming and also extraction is not • short time and more complete extraction
complete
•Not required skilled operator •Skilled operator is required
•For certain substances which are very less •Special attention should be paid on particle
soluble in solvent and requires only size of material and throughout process.
prolonged contact with solvent.
•Suitable method for less potent and cheap •Suitable method for potent and costly drugs
drugs

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 Soxhalation

Condenser

Side tube

Syphon Thimble
tube

Distillation flask

Heating Mantle

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  THE SOXHLET EXTRACTOR Continuous extraction of a
component from a solid mixture.
 Boiling solvent vapors rise up through the larger side-
arm. Condensed drops of solvent fall into the porous cup,
dissolving out the desired component from a solid
mixture.
 When the smaller side-arm fills to overflowing, it initiates
a siphoning action.
 The solvent, containing the dissolved component, is
siphoned into the boiler below residual solvent then
drains out of the porous cup, as fresh solvent drops
continue to fall into the porous cup.
 . . . and the cycle repeats . . .

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 Merits :
 Large amount of drug can be extracted with much smaller
quantity of solvent.
 Tremendous economy in terms of time, energy & ultimately
financial inputs.
 Small scale used a batch-process.
 Becomes more economical when converted into continuous
extraction.
 Procedure on large scale.
Demerits :
 Physical nature of drug.
 Solvent.
 Chemical constituent of drug.

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Supercritical Fluid Extraction
 For every substance, there is a critical temperature (Tc) and
pressure (Pc) above which no applied pressure can force the
substance into its liquid phase. If the temperature and pressure
of a substance are both higher than the Tc and Pc for that
substance, the substance is defined as a supercritical fluid.

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 Properties of SCFs :
 At the critical point, the density of the gas and liquid
phases is the same; there is no distinction between the
phases. i.e. between those of the pure liquid and gas.

 Supercritical posses densities that are liquid-like and

 Transport properties that are gas-like.

 These offers good penetrative ability and good

extractive ability.

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 Choice of SCFs solvent :

Good solving property,

Inert to the product,
Easy separation from the product,
Cheap,
Low CP because of economic reasons,
Carbon dioxide is the most commonly used SCF, due
primarily to its low critical parameters (31.1°C, 73.8 bar),
non-toxicity.

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 However, several other SCFs have been used in both
commercial and development processes. The critical
properties of some commonly used SCFs are ;

Critical Critical Pressure

Fluid
Temperature (K) (bar)
Carbon dioxide 304.1 73.8

Ethane 305.4 48.8

Ethylene 282.4 50.4

Propane 369.8 42.5

Propylene 364.9 46.0

Trifluoromethane
299.3 48.6
(Fluoroform)
Chlorotrifluoromethane 302.0 38.7

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Supercritical Fluid Extraction Process :
 The oldest typical and
most common supercritical
fluid extraction from solids is
performed as a batch process,
with a continuous flow of SCF.

 An extraction medium
(going to be SCF) stored in
the feed tank and liquid SCF
is pumped from a reservoir ;
it is heated and pressurized to
reach the supercritical conditions.

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Supercritical Fluid Extraction Process :
 Supercritical SCF enters the
extraction chamber where
contact with crude drug bed
occurs and the more volatile
substances are dissolved into
the supercritical fluid.
 Solute and SCF leave
extractor and extract is
precipitated in separators,
where SCF becomes
gaseous.
 Gas is recycled by
condensation before
returning to liquid reservoir.
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 Advantages of Supercritical Fluid
Extraction :
• Dissolving power of the SCF is controlled by pressure and/or
temperature.

• SCF is easily recoverable from the extract due to its volatility.

• Non-toxic solvents leave no harmful residue.

• High boiling components are extracted at relatively low temperatures.

• Separations not possible by more traditional processes can sometimes be

effected.

• Thermally labile compounds can be extracted with minimal damage as

low temperatures can be employed by the extraction.
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 Disadvantages of Supercritical Fluid
Extraction :

Elevated pressure required.

Compression of solvent requires elaborate recycling measures
to reduce energy costs.
High capital investment for equipment.

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 Applications of Supercritical Fluid
Extraction :
 Recovery of organics from oil shale
 Separations of biological fluids
 Bioseparation
 Petroleum recovery
 Crude dewaxing
 Coal processing (reactive extraction and liquefaction)
 Selective extraction of fragrances, oils and impurities from
agricultural and food products
 Pollution control
 Combustion and many other applications.

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 Counter-Current Extraction
 A liquid-liquid extraction process in which the solvent and
the process stream in contact with each other flow in opposite
directions.
 Screw extractors and carousel extractors are the two type
of equipments used for Counter-Current Extraction.

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 Counter-Current Extraction
PROCESS
• In counter-current extraction (CCE), wet raw material is

pulverized using toothed disc disintegrators to produce

fine slurry.
• The material to be extracted is moved in one direction
(generally in the form of fine slurry) within a cylindrical
extractor where it comes in contact with extraction
solvent.
• The further the starting material moves, the more
concentrated the extract becomes.
• Finally, sufficiently concentrated extract comes out at one
end of the extractor while the marc (practically free of
43 visible solvent) falls out from the other end.
 Advantages :

1. A unit quantity of the plant material can be extracted with

much smaller volume of solvent as compared to other methods
like maceration, decoction, and percolation.
2. CCE is commonly done at room temperature, which
spares the thermolabile constituents from exposure to heat
which is employed in most other techniques.
3. As the pulverization of the drug is done under wet
conditions, the heat generated during comminution is
neutralized by water. This again spares the thermolabile
constituents from exposure to heat.
4. The extraction procedure has been rated to be more
efficient and effective than Continuous hot extraction.
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 Applications :

1. DNA purification:
2. Food Industry:
3. Ex. Citrus oils, Unsaturated fatty acids, and squalene
tocopherol.
An important application is citrus oil processing,
An important subject in perfumes and food industries.

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 Microwave-assisted Extraction :
Microwaves are electromagnetic radiations with a
frequency from 0.3 to 300 GHz (Camel, 2001).
In order to avoid interferences with radio
communications, domestic and industrial microwaves
generally operate at 2.45 GHz (Fig. 1). Owing to their
electromagnetic nature, microwaves possess electric and
magnetic fields which are perpendicular to each other.
The electric field causes heating via two simultaneous
mechanisms, namely, dipolar rotation and ionic
conduction

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 Microwave-assisted extraction offers a rapid delivery of energy
to a total volume of solvent and solid plant matrix with
subsequent heating of the solvent and solid matrix, efficiently and
homogeneously.
 Components of the sample absorb microwave energy in
accordance to their dielectric constants.
 When plant material is immersed inside a microwave transparent
solvent, the heat of microwave radiation directly reaches to the
solid without being absorbed by the solvent, resulting in
instantaneous heating of the residual moisture in the solid.
 Heating causes the moisture to evaporate and creates a high
vapour pressure that breaks the cell wall of substrate and
releases the content into solvent.
 The extracting selectivity and the ability of the solvent to interact
with microwaves can be modulated by using mixtures of
solvents.
 One of the most commonly used mixtures is hexane-acetone.
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48
 Advantages of Microwave Assisted
Extraction :
It reduces solvent consumption,
It has a shorter operational time,
It possess moderately high recoveries,
Has a good reproducibility and minimal sample
manipulation for extraction process.

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 Disadvantages of Microwave Assisted
Extraction:
An additional filtration or centrifugation is
necessary to remove the solid residue during
MAE.
Furthermore, the efficiency of microwaves can be
very poor when either the target compounds or the
solvents are non-polar, or when they are volatile.

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 Applications of Microwave-Assisted
Extraction:
MAE can extract nutraceuticals products
from plant sources in a faster manner than
conventional solid–liquid extractions.
MAE (80% methanol) could dramatically reduce
the extraction time of ginseng saponin from 12 h
using conventional extraction methods to a few
seconds.

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  Biologically active compounds extracted by microwave-
assisted Technique
• Extraction of taxanes from Taxus brevifolia needles,
• Azadiractin related limonoids from Azadirachta indica seed
kernels,
• Extraction of glycyrrhizic acid from Glycyrrhizia glabra roots,
• Extraction of artemisinin from Artemisia annua.
 A higher microwave temperature and a short extraction time
are more effective in extracting anti-oxidative phenolic
compounds from tomato using MAE.
 MAE was proven as a potential alternative to traditional
methods for extraction of phenols such as chlorogenic acids
from green coffee beans.
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 Ultrasonication-Assisted Extraction:

The procedure involves the use of ultrasound waves, which have

frequencies higher than 20 kHz, have great effects on extraction
yield and kinetics.

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 UAE involves ultrasonic effects of acoustic cavitations. Under
ultrasonic action solid and liquid particles are vibrated and
accelerated and, because of that solute quickly diffuses out from
solid phase to solvent
Ultrasound assisted extractors are ultrasonic baths or closed
extractors fitted with an ultrasonic horn transducer. The
mechanical effects of ultrasound induce a greater penetration of
solvent into cellular materials and improve mass transfer.

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 Advantages of Ultra sonicated
extraction:
It is an inexpensive, simple and efficient alternative to
conventional extraction technique.
It include the increase of extraction yield and faster kinetics.
It reduce the operating temperature allowing the extraction of
thermolabile compounds.
Compared with other novel extraction techniques such as
microwave-assisted extraction, the ultrasound apparatus is
cheaper and its operation is easier.

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 Disadvantages of Ultra sonicated
extraction:
The active constituents of medicinal plants through formation of
free radicals and consequently undesirable changes in the drug
molecules.

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 Applications:
 Used to extract nutraceuticals from plants such as essential oils and
lipids dietary supplements.
e.g. oils from almond, apricot and rice bran
 Extraction of saponinfrom ginseng, the observed total yield and
saponin yield increased by 15 and 30%, respectively
 extracts. It was found that rice bran oil extraction can be efficiently
performed in 30 min under high-intensity ultrasound either using
hexane or a basic aqueous solution.
 Extraction rates of carvone and limonene by ultrasound-assisted
extraction with hexane were 1.3–2 times more rapid than those by
the conventional extraction depending on temperature

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 Conclusion:
 Extraction is essential for isolation of different chemical
constituent from crude drug material.
 Extraction depends on properties of material to be
extracted. Hence it is necessary to study extraction methods
in detail.

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 SOLVENTS

Petroleum ether :- Fixed oils, Phytoglycerols.

Benzene:- Fixed oils, Phytosterols.
Chloroform;- Alkaloids
Acetone:- Phytosterols
Ethanol:- Carbohydrates, Glycosides
Saponin:- Phenolics, Tannins, proteins, Amino
acids
Water:- Proteins, Amino acids, Glycosides, Gums,
Mucilages, Carbohydrates
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 properties of ideal solvent:

1.Be highly selective for the compound to be extracted.

2.Have a high capacity for extraction in terms of
coefficient of saturation of the compound in the
medium.
3.Not react with the extracted compound or with other
compounds in the plant material.
4.Have a low price.
5.Be harmless to human being and to the environment.
6.Be completely volatile.

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  DIFFICULTIES:-
Different active constituents like alkaloids, glycosides, tannins,
terpenoids, resins oils etc requires advanced knowledge of
phytoconstituents which help in selection of method.
Different forms of insoluble matters may affect the extraction
process.
eg. Cellulose, proteins etc. in many drugs only the active
constituent is not soluble material but along with it large
proportion of unwanted material is solubilized. In such
situations, a solvent chosen is as selective as possible.
Wet vegetable material is an excellent medium for microbial
growth and it may leads to loss of active substances and solvent
must have suitable preservative action.
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Reference :
1. Mukharji Pulok K. 2002,Quality Control of Herbal Drugs,1st
edition Published by Business Horizon, p.p 380-421.
2. Mehta R.M. 2010, Introduction to Pharmaceutics ,5th edition
Published by Vallabh Prakashan, p.p150-167.
3. Rangari v.d. 2002 ,Pharmacognosy and Phytochemistry ,1st
edition ,volume 1st Published by Career Publication, p.p.95-98
4. Cooper J.W, Gunn`s Colin 2010-2011, Register of General
Pharmacy p.p.308-393
 Reference :
5. Be´Atrice, K. and Philippe, C. 2002, Recent Extraction
Techniques for NaturaProducts:Microwave-assisted
Extraction and Pressurised solvent Extraction.
PHYTOCHEMICAL ANALYSIS, 13 pp. 105-113.
6.Bhadoriya, U., Tiwari, S., Mourya, M. and Ghule, S. 2011.
Microwave-Assisted Extraction of Flavonoids from
Zanthoxylum Budrunga w. Optimization of Extraction
Process. Asian Journal of Pharmacy and Life Science, Vol.
1 (1), pp. 82-83. [Accessed: 20 Sep 2013].

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