DECOCTION AND HOT

CONTINUOUS EXTRACTION
TECHNIQUES

Sudeep Tandon
Scientist
Chemical Engineering Division
CIMAP, Lucknow

INTRODUCTION

¾ Decoction is a water-based preparation to extract

active compounds of herbs, made by boiling the
plant parts for some period.
¾ Used to primarily extract the mineral salts and
bitter principles of plants, rather than vitamins and
volatile ingredients
¾ It is a liquid preparation made by boiling the herbs
with water, differing from infusions that the latter
are not actively boiled
¾ Decoctions are usually the method of choice when
working with tougher and more fibrous plants,
barks and roots (and which have water soluble
chemicals).

1
• Instead of just steeping it in hot water, the plant
material is boiled for a longer period of time to soften
the harder woody material and release its active
constituents
• The plant materials are generally into broken into
small pieces or grounded into a powder—the smaller
they are, the more easily they will be absorbed into
the water
• More heat is needed in making decoctions than
infusions, since mostly the parts of the herb that are
used in decoctions—the bark and roots—are very
dense in nature.
• Unfortunately, the high heat does tend to destroy
some of the herb's volatile oils.

Methods of preparing decoctions

Different methods have been described in

literature for preparation of decoctions…

2
 METHOD FOR PREPARING DECOCTIONS IN TSM /
AYURVEDA
• Traditionally known as ‘KWATHA’
• Methodology : The Drug in form of ‘Yavakuta’ (small pieces
taken in earthen pots or tinned cooper vessel with clay on
outside
If drug is soft- 4 times water
If drug is moderately hard – 8 times water
If drug is very hard – 16 times water
• Then boiled on low flame till reduced to
1/4th in case of soft drugs
1/8th in case of moderately or very hard drugs
• Cooled, strained and filtrate collected in clean vessels

IN ANOTHER METHOD DESCRIBED ELSEWHERE …….…

™ To prepare a decoction, select a ceramic pot (Material can vary) with
a snug fitting lid.
™ Measure the amount of herb needed into the pot and add the proper
amount of cold water depending on how many cups of the decoction
you wish to prepare.
™ Turn on the heat to medium high and bring to a boil. Place the lid
on the pot and reduce the heat to medium or medium-low so that the
mixture stays at a good simmer.
™ Simmer it covered for certain fixed time or till volume of water
reduces to fixed ratios
™ Remove from heat and cool slightly. If using cut herbs, strain the
mixture through a strainer
™ When straining, make sure to press on the cut herb pieces in the
strainer to get as much liquid/decoction out of the herb pieces as
possible.
™ If using powdered herb, allow the powder to settle to the bottom of
the pot and then pour off the decoction from the top

3
 STRONG DECOCTIONS

• Depending on the type of plant material used, strong

decoctions are prepared in two general ways.
• The first involves boiling the mixture longer. This is
usually indicated when working with larger woody pieces
of bark. Longer boiling time, up to 2 hours or more, is
sometimes necessary to break down, soften, and extract the
larger pieces.
• Alternatively, when smaller woody pieces are used yet a
stronger remedy is wanted, the decoction is prepared as
above (boiling 20 minutes), then it is allowed to sit/soak
overnight before straining out the herb.

• Only Recently prepared decoctions should be dispensed

• Decoctions should be stored under refrigerated conditions
• The drug concentration of a decoction should be well specified for
the plant material or should be prescribed by a physician

If drug concentration is not specified then following general formula of USP

XII can be used
• The Drug, coarsely comminuted …………….. = 50 gm
• Water, sufficient quantity………………...to make 1000 ml
Method
• Place the drug in a suitable vessel provide with a cover
• Pour upon t 100 ml of cold water, cover it and boil for about 15 min
• Allow to cool to 40oC
• Strain and use as such or dilute again to 1000 ml

4
 Extraction with Volatile solvents
Mainly applied for
9 Medicinal plants /herbs for preparation of standardized
extracts / total crude extracts like alkaloids, saponins,
glycosides etc
9 Extracts which contain bio active constituents for further
downstream processing and isolation of the pure
phytomolecules
9 Aromatic plants mostly florals like rose, jasmine,
tuberose for preparation of concretes and absolutes
9 Spices or spice plants for preparation of the oleoresins /
resenoids

5
9 Solvent Extraction of herbs fall in category of solid liquid
extraction and is also referred as the leaching process
9 Leaching is the process of removing a solute from a solid by the
use of a liquid solvent.
9 The separation usually involves selective dissolution, with or
without diffusion.
9 Lixiviation is also used less frequently as a synonym for
leaching
9 The insoluble solid may be massive and porous; more often it is
particulate, and the particles may be openly porous, cellular
with selectively permeable cell walls, or surface-activated.
9 The stream of solids being leached and the accompanying
liquid is known as the underflow
9 The solid content of the stream is sometimes called marc.
9 The stream of liquid containing the leached solute is the
overflow

PRINCIPLE OF SOLVENT EXTRACTION

• When solvent penetrates into plant material it is necessary, to verify the
diffusion process. i.e. the mass transfer of the product from the solid phase to the
liquid.
• The rate of mass (Δ m) transfer in the time dt is a function of surface contact
between the phases (S), of the coefficient diffusion of the solute in the solution
(D) and of the concentration of the solute in the liquid (C) to the time t and in
the liquid film around the solid that we are extracting (Cs) as well as the
thickness of the liquid film around the solid matrix (S).
ΔM = SD (Cs – C)
s
Concept of Equilibrium

• The practical interpretation of leaching equilibrium is the state in which

the overflow and underflow liquids are of the same composition; on a y-x
diagram, the equilibrium line will be straight line through the origin
with a slope of unity.
• It is customary to calculate the number of ideal (equilibrium) stages
required for a given leaching task

6
TWO STEPS ARE ALWAYS INVOLVED IN SOLID LIQUID
EXTRACTION
1. Contact of liquid solvent with the solid to effect transfer of
solute from the solid to the solvent.
2. Separation of resulting solution from the residual solid.
Two other auxiliary operation are involved namely :
a) Preparation of the solid for extraction and
b) Recovery of solute form the solvent, usually by evaporation
or distillation of solvent from the solute
MECHANISMS OF EXTRACTION
Single Stage Extraction :

FRESH SOLVENT OVERFLOW SOLUTION

EXTRACTION
STAGE
SOLID UNDERFLOW SOLID FEED

Multistage Co current Extraction

Fresh Solvent Fresh Solvent

Fresh Solvent
Extraction Extraction
Extraction
Stage 2 Stage n
Stage 1
Solid Feed Solid Under flow
Overflow Solution Overflow Solution
Overflow Solution
Multistage Counter current Extraction

Fresh Solvent
Overflow Solution
Extraction Extraction Extraction
Stage1 Stage 2 Stage n
Solid Feed
Solid Under flow

7
 PROCESS PARAMETERS EFFECTING SOLID
LIQUID / SOLVENT EXTRACTION

• MATRIX CHARACTERISTICS
• CHOICE OF SOLVENT
• METHOD OF CONTACTING
• TEMPERATURE OF EXTRACTION
• NUMBER OF WASHES
• CONDITIONS FOR EXTRACTION-AGITATION

MATRIX CHARACTERSTICS
¾ Solvent extraction strongly depends on matrix characteristics and
particle size as the internal diffusion may be limiting step during
extraction.
¾ Many pharmaceutical products recovered from plant roots, stems and
leaves, the plant material is frequently dried before treatment, and
these does much toward rupturing the cell walls and releasing the solute
for direct action by the solvent.
¾ The cells are, of course smaller than this, but they are largely ruptured
by the flaking process, and constituents are then more rapidly contacted
by the solvent.
¾ The degree of comminution required will also depend on the
composition of the crude drug e.g.
is it hard or soft ?,
is it thick or thin ?
¾ If the drug is leaves or petals then it will be easily penetrated by the
solvent, therefore the degree of comminution need not be great, whereas
hard and woody substances will require a greater reduction in size.

8
CHOICE OF SOLVENT :

¾ Selectivity : β = Wt fraction of solute in Residue

Wt fraction of solute in Extract
Selectivity must exceed unity (i.e. > 1) the more so better.

¾ Insolubility / Miscibility of Solvent

¾ Low boiling point and high volatility for better Recoverability
Polarity
¾ Solvent should be non toxic
¾ Non flammable & low cost
¾ Non Denaturing nature
¾ Chemically non-reactive towards the product being extracted
¾ ECOFREINDLY

9
 SOME COMMON SOLVENTS USED FOR EXTRACTION OF MAP’S
Solvent BP (OC) Miscibility with H2 O TLVb
Acetone 56 ∞ 1000
Aceric Acid 116-117 ∞ 10
Ethyl Acetate 77 80 400
Benzene 80 T 25
Buthan-2-one 79.5 19 2200
Cyclohexane 80.7 T 300
Dichloromethane 39.7 1.3 2200
Chloroform 61 8 50
Carbon tetrachloride 76.77 0.8 10
Hexane 69 T -
Ethanol 78 ∞ 1000
Ethyl ether 34.6 1.2 400
Petrol ether 30-50 - 500
Propantriole 290* ∞ -
Methanol 64.7 ∞ 200#
1-propanol 91 M 400
2-propanol 82.4 M? 400
tolune 110.6 0.06 100#

b - p.p.m .t = < 0.01%, * = with decomposition; m = miscible,∞ = completely miscible

TLV : Threshhold Limit Values

TEMPERATURE

¾ Higher temperatures results in greater solubility of solvents and

and
therefore are sometimes desirable to realize higher solute
concentration in the extract.
¾ The temperature of the extraction should be chosen for the best
balance of solubility, solvent-
solvent-vapor pressure, solute diffusivity,
solvent selectivity, and sensitivity of product.
¾ Elevated temperature, in case of some natural materials may
result in excessive extraction of undesirable material.
¾ Use of high temperature during extraction is avoided when the
active constituents are thermo labile or volatile and to reduce the
level of unwanted constituents.
¾ Higher temperature operation may also not be permissible
because of solvent losses and for safety consideration.
consideration.

10
 METHOD OF SOLID LIQUID CONTACTING

™ In fixed bed contacting, the solid particle are stationary,

™ While dispersed contact involve motion of solid particles
relative to each other and also relative to liquid.
™ Solvent may be contacted with a fixed bed of solids in three
different ways:
1) Spray Percolation
2) Full immersion
3) Intermediate drainage.

Solid – Liquid Extraction: Equipments

Can be divided into two main classes :

1) Those in which the leaching is accomplished by percolation

(Passing the solvent through a bed of static particulate material)

2) Those in which particulate solid are dispersed into a liquid and

subsequently separated from it.

EACH CAN BE EITHER BATCH AND CONTINUOUS

UNITS.

11
 PERCOLATION

¾ Percolation is generally carried out in batch

tanks and in continuous or dump extractors
(usually on smaller scale).

COLD PERCOLATION :

¾ This method allows processing of the herbs

into a liquid extract without utilizing heat or
concentration, both of which may cause
damage to the constituent of the whole herb.
It is referred to as soft extraction technique.

HOT PERCOLATION :

In this method the bio-mass is added to the

container containing the solvent and the
mixture is heated under reflux. The technique
is sometimes referred to as total extraction.

BATCH PERCOLATORS

¾ The batch tank is not unlike a big nutsche filter; it is a large

circular or rectangular tank with a false bottom.
¾ The solids to be leached are dumped into the tank to a uniform
depth.
¾ They are sprayed with solvent until their solute content is reduced
to an economic minimum and are then excavated.
¾ Countercurrent flow of the solvent through a series of tanks is
common, with fresh solvent entering the tank containing most
nearly exhausted material.

CONTINUOUS PERCOLATORS
¾ Coarse solids are also leached by percolation in moving-bed
equipment, including single-deck and multideck rake classifiers,
bucket-elevator contactors, and horizontal-belt conveyors.

12
 Vessels with Agitation

• Channeling of the solvent in percolation of

fixed bed, with its consequents slow and
incomplete leaching, can be avoided by
stirring the liquid and solid in leaching vessel.
• The agitation vessel is generally used for
coarse solids
• This device is operated in batch wise fashion
and provides a single leaching stage.

Percolation Vs. Agitation

• If a solid in the form large lumps is to be leached, a decision must frequently be
made whether to crush it coarse lumps and leach by percolation or whether to
grind it fine and leach by agitation
• Fine grinding is more costly but provides more rapid and possibly more
thorough leaching.
• Coarsely ground particles, on the other hand .Leach more slowly and possibly
less thoroughly but on draining may retain relatively little solution., require
less washing, and thus provide a more concentrated final solution.
• Leaching is generally more efficient in a thoroughly agitated vessel then by
percolation, probably because the large amount of static liquid holdup makes
important amounts of solute unavailable.
• Agitation operates in stage wise or in continuous- contact fashion.
• Stage wise equipment is sometimes assembled in multiple units to produce
multistage effects, whereas continuous-contact equipment may provide the
equivalent of many stages in a single device.

13
 SOXHLET EXTRACTOR
Soxhlet extractor : a bench scale Laboratory
apparatus invented in 1879 by Franz von
Soxhlet.

¾ Classical technique for the solvent extraction

of nutraceuticals from plant matrices
¾ The plant material is placed in a thimble-
holder, and filled with condensed fresh solvent
from a distillation flask.
¾ When the liquid reaches the overflow level, a
siphon aspirates the solution of the thimble-
holder and unloads it back into the distillation
flask, carrying extracted solutes into the bulk
liquid.
¾ In the solvent flask, solute is separated from the
solvent using distillation.
¾ Solute is left in the flask and fresh solvent
passes back into the plant solid bed.
¾ The operation is repeated until complete A schematic representation of
extraction is achieved. a Soxhlet extractor

Advantages and disadvantages of Soxhlet Extraction

Advantages :
¾ The displacement of transfer equilibrium by repeatedly bringing fresh
solvent into contact with the solid matrix.
¾ Maintaining a relatively slightly high extraction temperature with heat from
the distillation flask.
¾ No filtration requirement after leaching. Also, the Soxhlet method is
very simple and cheap.

Disadvantages :

¾ The extraction time is long.

¾ Agitation can not be provided in the Soxhlet device to accelerate the
process.
¾ The large amount of solvent used requires an evaporation concentration
procedure.
¾ The possibility of thermal decomposition of the target compounds can
not be ignored
¾ As the extraction usually occurs at the boiling point of the solvent for a long
time

14
 LARGE SCALE CONTINUOUS TYPE EXTRACTORS

¾ The Bollman-type extractor.

¾ Rotocel extractor.
¾ Kennedy extractor.
¾ Screw-Conveyor Extractors.
¾ Hildebrandt total-immersion extractor.

Most of the above type extractors find applications in the

metallurgical industries for ore extraction and leaching.
Some extractors however have been used for vegetable oil extractions

15
 ACCELERATED SOLVENT EXTRACTION
Accelerated solvent extraction (ASE) is a solid–liquid extraction process
performed at elevated temperatures, usually between 50 and 200oC and at
pressures between 10 and 15 MPa
Accelerated solvent extraction is form of pressurized solvent extraction
that is quite similar to SFE.
Extraction is carried out under pressure to maintain the solvent in its
liquid state at high temperature.
Technique still in experimental stages

ADVANTAGES AND DISADVANTAGES OF ASE

ADVANTAGES
¾ Use of non toxic extracting solvents such as carbon dioxide and
water has economic and environmental benefits.
¾ Accelerated Solvent extraction is considered as a potential
alternatives technique to SFE for extraction of polar compound.
¾ Compared with traditional Soxhlet extraction, there is a dramatic
decrease in the amount of solvent and the extraction time for ASE

DISADVANTAGES

¾ Accelerated solvent extraction performed with high extraction

temperature, which may lead to degradation of thermo labile
compounds.

16
 LIQUID LIQUID EXTRACTION
SEPARATION OF A COMPONENT FROM A LIQUID MIXTURE BY TREATMENT
WITH A SOLVENT IN WHICH THE DESIRED COMPONENT IS PREFERENTIALLY
MORE SOLUBLE.
Solvent : The liquid with which the feed is contacted with.
Extract : The solute rich solvent product of the operation.
Raffinate : Residual liquid from which solute has been removed.
In liquid liquid extraction the products recovered have to be subjected to further
MT operations like distillation, crystallization, chromatography etc. for final
recovery.
SOLVENT

FEED May be batch or continuous

Mixer Settlers e.g. Kerr-Mcgree
Extractor

SINGLE STAGE EXTRACTION

EXTRACT

MULTI STAGE EXTRACTION

FEED RAFFINATE
RAFFINATE

MIXER MIXER MIXER RAFFINATE

SEPARATOR SEPARATOR SEPARATOR
SOLVENT 1 2 ‘n’

SOLVENT SOLVENT

EXTRACT EXTRACT EXTRACT

CO-CURRENT FLOW EXTRACTION SYSTEM

RAFFINATE RAFFINATE DEPLETED

MIXER MIXER MIXER
RAFFINATE
FEED SEPARATOR SEPARATOR SEPARATOR
1 2 ‘n’
SOLVENT

SOLVENT
ENRICHED COUNTER CURRENT FLOW EXTRACTION SYSTEM
WITH
PRODUCT

• Rotating Disc Contactors

Different types of
liquid liquid
extraction columns
• Perforated Plate ( Karr Column)
• Pulsed Plate Columns
• Scheibel Extractors
• Centrifugal Counter current “ Podbielniak Extractor”

17
 HORIZONTAL LIQUID LIQUID VERTICAL RECIPROCATING LIQUID
‘PODBIELNIAK EXTRACTER LIQUID EXTRACTION “ KARR”
COLUMN

In Industry Solvent Extraction

units for MAPs is based on
‘Soxhlet principle with
recycling of solvents

Basic equipments of an extraction

unit consists of

• Drug holders / Extractors

• Solvent Storage Vessel
• Reboiler Kettle
• Condensers
• Breather system
• Infrastructure
• Boiler
• Refrigerated Chilling unit
• Vacuum
• Inert Gas
LARGE SCALE SOLVENT EXTRACTION UNIT

18
DESIGNING A SOLVENT EXTRACTION PLANT
FOR HERBS !
High Efficiency of Extraction
Minimal Solvent losses IMPORTANT
Facility for cold / hot extraction FACTORS WHILE
Extraction with agitation SETTING UP AN
EXTRACTION
Multiple solvent extraction system UNIT
Multiple fraction collection
Online filtration unit
Solvent recycling and condensing unit
Vent lines with breather for minimizing solvent losses and safety
Brine circulation unit
Fractionating column for separation of solvent mixtures
Efficient evaporating systems like falling film, wiped film or rotary
evaporators to work under low pressures
Vacuum systems with cold traps
GMP Compatible : All Stainless Steel units

19
 Condenser
Recovered
Solvent

JasmineFlowers Cooling
Water
Solvent
ToVacuum

Percolation Vacuum
Vessel Concentr
Steam
ator

Perforated Grid

Extract
Line Filter
Rotary Vacuum Jasmine
Evaporator Concrete

Filtratio Absolute
Jasmine Absolute n Chilling
Plant
Alcohol

Production of jasmine absolute using solvent extraction technique

SOME IMPORTANT MEDICINAL PLANTS & THEIR ACTIVE CONSTITUENTS

(That are extracted / isolated by Solvent Extraction technique)
Plant Useful Plant Active Constituent Major Use
Part
Artemesia annua (Quinghasou) Whole Plant Artemisinin Antimalarial
Cassia augustifolia (senna) Leaves, Pods Sennosides A & B Laxative
Cantharanthus roseus Roots Ajmalcine,Vinblastine Anticancer
(Periwinkle) Leaves Vincrystine
Chyrysanthemum Flowers Pyrethrins Insecticidal
cinerariaefolium (Pyrethrum)
Rauvolifolia serpentine Roots Resperine, Rescinnamine Hypertensive
Sedative
Withania somniferum Roots Somniferum, Phytosterol Stimulant
Antiinflamatory
Ammi majus Seeds Xanthotoxin Skin diseases
Leucoderma
Andrographis panniculata Leaves Di terpenoids Hepatprotective
Andrographalides
Gloriosa superba Rhizomes Colchicine Gout,
Rheumatism
Aesculus indica Seeds Aescin Anti
inflammatory
Centella asiatica Whole Pant Asiaticosides Tonic
Aspatic acid Stimulant
Bacopa munnerai Whole plant Baccosides Tonic
Stimulant
Dioscoria deltoidea Rhizomes Diosgenin Steroid

20
 SOLVENT EXTARCTION PLANT

SOLVENT EXTARCTION PLANT FOR MAP’S AT BIOTECH PARK

LUCKNOW

21
DRUG HOLDERS / EXTRACTORS

22