11/14/16

COLLEGE   OF  PHARMACY
UNIVERSITY  OF  BASRAH

Extraction;;  maceration  
and  percolation  
By
Dr.  Mohammed  Sattar
2016/2017

COLLEGE  OF   PHARMACY

UNIVERSITY  OF  BASRAH

Outlines
ØExtraction
ØMethod  selection  
ØMaceration
ØPercolation

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Extraction Methods for Preparing Solutions

vThe sole purpose of such basic extraction procedures for crude drugs are to
obtained the therapeutically desirable portion and eliminate the inert material
by treatment with a selective solvent known as the Menstruum.

vCertain pharmaceutical preparations are prepared by extraction, that is, by

withdrawal of desired constituents from crude drugs through the use of
selected solvents in which the desired constituents are soluble.

vTypes of extraction procedures play a decisive role for the qualitative and
quantitative composition of the extracts.

vThe standardized extracts, thus obtained are further processed for inclusion in
other dosage forms such as Tablets and Capsules containing several groups of
plant’s metabolites.

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vBecause each crude drug contains a number of constituents that may be

soluble in a given solvent, the products of extraction, termed extractives, do
not contain just a single constituent but rather varying constituents, depending
on the drug used and the conditions of the extraction.

vTinctures, fluidextracts, and extracts are the pharmaceutical products most

commonly prepared from extractives.

vThe solvent systems used in extraction are selected on the basis of their
capacity to dissolve the maximum amount of desired active constituents
and the minimum amount of undesired constituents.

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vIn drug extraction, the solvent or solvent mixture is referred to as the

menstruum, and the plant residue, which is exhausted of active
constituents, is termed the marc.
vThe selection of the menstruum to use in the extraction of a crude
drug is based primarily on its ability to dissolve the active
constituents.

vAlthough water and alcohol and to a lesser extent glycerin are

probably the most frequently employed solvents in drug extraction,
acetic acid and organic solvents like ether may be used for special
purposes.

COLLEGE  OF   PHARMACY

UNIVERSITY  OF  BASRAH

Methods of Extraction

(1)Maceration
(2) Percolation
(3) Decoction
(4) Digestion
(5) Infusion

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COLLEGE  OF   PHARMACY

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Methods of Extraction
• The principal methods of drug extraction are maceration and
percolation.

• Factors affecting method selection:

1. The nature of the crude drug,
2. The drug adaptability to each of the various extraction methods, and
3. The interest in obtaining complete or nearly complete extraction of the
drug.

COLLEGE  OF   PHARMACY

UNIVERSITY  OF  BASRAH

Character  of  Drug

Ø If  hard  and  tough  (such  as  nux vomica)  use  percolation.  
Ø If  soft  and  parenchymatous (such  as  gentian)  use  maceration.
Ø If  ‘unpowderable’  (such  as  squill)  use  maceration.  
Ø If  an  ‘unorganized  drug  (such  as  benzoin)  use  maceration.  
Ø If  preferable  to  avoid  powdering  (such  as  senna fruits)  use  
maceration.  
Thus,  knowledge  o f  the  p harmacognosy of  the  d rug  is  
essential  to  selection  o f  the  extraction  p rocess  that  will  g ive  
the  b est  results  

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Therapeutic   value  of  the  drug  

• When  the  drug  has  considerable  therapeutic  value,  the  
maximum  extraction  is  required,  so  that  percolation  is  used,  as  
in  belladonna.  
• If  the  drug  has  little  therapeutic  value,  however,  the  efficiency  of  
extraction  is  unimportant  and  maceration  is  adequate;;  for  
example,  “flavours”  (lemon),  or  “bitters”,  (gentian).  

COLLEGE  OF   PHARMACY

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Stability  o f  d rug  
• Continuous  extraction  should  be  avoided  when  the  constituents  of  the  
drug  are  thermo-­labile.  

Solvent
• If  the  desired  constituents  demand  a  solvent  other  than  a  pure  boiling  
solvent  or  an  azeotrope,  continuous  extraction  should  be  used.  

• Recovery  o f  solvent  from  the  marc  

• The  residue  of  the  drug  after  extraction  (often  known  as  the  marc)  is  
saturated  with  solvent  and  if  economic  the  latter  is  recovered.  

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Cost  of  drug  

ØFrom  the  economic  point  of  view,  it  is  desirable  to  obtain  
complete  extraction  of  an  expensive  drug,  so  that  percolation  
should  be  used;;  Ginger  is  an  example.  

ØFor  cheap  drugs,  the  reduced  efficiency  of  maceration  is  

acceptable  in  view  of  the  lower  cost  of  the  process.  In  particular,  
the  cost  of  size  reduction  to  a  powdered  state  is  avoided,  
whereas  this  is  a  significant  part  of  the  percolation  process.  

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Concentration   of  product  
• Dilute  products  such  as  tincture  can  be  made  by  maceration  or  
percolation,  depending  on  the  previous  factors.

• For  semi-­concentrated preparations  (concentrated  infusions,  for  

e.g.)  the  more  efficient  percolation  process  is  used)  unless  the  
drug  cannot  be  powdered  or  is  not  worth  powdering,  when  double  
or  triple  maceration  is  chosen.  

• Concentrated  preparations,  of  which  liquid  extracts  or  dry  extracts  

are  example,  are  made  exclusively  by  percolation,  with  the  
exception  that  continuous  extraction  can  be  used  if  the  solvent  is  
suitable  and  the  constituents  are  thermo-­stable  
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COLLEGE  OF   PHARMACY

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(1) Maceration: Steady state extraction

• Term derived from Latin word
“macerare” meaning to soak.

• It is a process in which the properly

comminuted drug is permitted to soak
in the menstruum until the cellular
structure is softened and penetrated
by the menstruum and the soluble
constituents are dissolved.

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• For drugs containing little or no cellular material, such as

benzoin, aloe, and tolu, which dissolve almost completely in
the menstruum, maceration is the most efficient method of
extraction.

• Maceration is usually conducted at a temperature of 15℃ to

20 ℃ for 3 days or until the soluble matter is dissolved.

• Examples:
1. Compound Benzoin,
2. Sweet orange Peel Tincture;;
3. Compound Cardamon;;
4. Tolu Balsam Tincture

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Plant Material:  cut  into  small  pieces

Placed  in  a  closed  vessels  with  
menstruum  
Standing  with  occasional shaking

Liquid strained  off  and  clarified  

Evaporation  and  concentration 15

COLLEGE  OF   PHARMACY

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Modifications  of  the  General  Processes  of  Maceration  

• Repeated  maceration  may  be  more  efficient  than  a  single  maceration,  
since  an  appreciable  amount  of  active  principle  may  be  left  behind  in  the  
first  pressing  of  the  marc.  
• The  repeated  maceration  is  more  efficient  in  cases  where  active  
constituents  are  more  valuable.  
• Double  maceration  is  used  for  concentrated  infusions  which  contain  
volatile  oil,  e.g.  Concentrated  Compound  Gentian  Infusion.  
• Where  the  marc  cannot  be  pressed,  a  process  of  triple  maceration is  
sometimes  employed.  
• The  total  volume  of  solvent  used  is  however  large  and  the  second  and  
third  macerates  are  usually  mixed  and  evaporated  before  adding  to  the  
first  macerates.  
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COLLEGE  OF   PHARMACY

UNIVERSITY  OF  BASRAH

• This  precludes,  the  use  of  the  process  for  preparations  containing  
volatile  ingredients.  
• In  a  few  cases,  it  is  desirable  to  change  the  physico – chemical  nature  
of  the  solvent  during  a  single  maceration  process.  
• Opium  Tincture  is  prepared  by  using  change  of  the  physico-­ chemical  
nature  of  the  solvent  as  indicated  below:  

The  addition   of  
Sliced  opium   90%  Alcohol   is  
alcohol  prevent  
disintegrated in   added  to  the  cold  
the  formation  of  
boiling  water  and   mix  and  macerate  
gummy  matrial in  
left  to  cold  for  6h for  24h
the  final  product.
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Circulatory  extraction
• The  efficiency  of  extraction  in  a  maceration  
process  can  be  improved  by  arranging  for  the  
solvent  to  be  continuously  circulated  through  the  
drug.  
• Solvent  is  pumped  from  the  bottom  of  the  vessel  
to  the  inlet  where  it  is  distributed  through  spray  
nozzles  over  the  surface  of  the  drug.  
• The  movement  of  the  solvent  reduces  boundary  
layers,  and  the  uniform  distribution  minimizes  
local  concentration  in  a  shorter  time.
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COLLEGE  OF   PHARMACY

UNIVERSITY  OF  BASRAH

Multiple  stage  extraction

• Like  the  normal  maceration  process,  
• however,  extraction  is  incomplete,  since  mass  transfer  will  
cease  when  equilibrium  is  set  up.  This  problem  can  be  
overcome  by  using  a  multistage  process.
• The  equipment  needed  for  this  method  is  a  circulatory  
extractor  connected  to  number  of  tanks  to  receive  the  
extracted  solution.  

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COLLEGE  OF   PHARMACY

UNIVERSITY  OF  BASRAH

Procedures
1. Fill  extractor  with  drug,  add  solvent  to  circulate.  Run  off  to  receiver  1.
2. Refill  extractor  with  solvent  and  circulate.  Run  off  to  receiver  2.  
3. Refill  extractor  with  solvent  and  circulate.  Run  off  to  receiver  3.  
4. Remove  drug  from  extractor  and  recharge.  Return  solution  from  1  to  
extractor.  Remove  for  evaporation.
5. Return  solution  from  2  to  extractor  and  circulate.  Run  off  to  receiver  1  
6. Return  solution  from  3  to  extractor  and  circulate.  Run  off  to  receiver  2  
7. Add  fresh  solvent  to  extractor  and  circulate.  Run  off  to  receiver  3  
8. Remove  drug  from  extractor  and  recharge.  Repeat  cycle.  
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Advantages
1. The  drug  is  extracted  as  many  times  as  there  are  
several  receivers.
2. The  last  treatment  of  the  drug  before  it  is  discharged  is  
with  fresh  solvent,  giving  maximum  extraction.
3. The  solution  is  in  contact  with  fresh  drug  before  
removal  for  evaporation,  giving  the  highest  possible  
concentration.  
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COLLEGE  OF   PHARMACY

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(2) Percolation: Exhaustive extraction

• The  term  percolation,  from  the  L atin  p er,  
meaning  through,  and  colare,  meaning  to  strain.

• It  may  be  described  g enerally  as  a  p rocess  in  

which  a  comminuted  d rug  is  extracted  o f  its  
soluble  constituents  b y  the  slow  p assage  o f  a  
suitable  solvent  through  a  column  o f  the  d rug.

• The    drug  is  p acked  in  a  special  extraction  

apparatus  termed  a  p ercolator,  with  the  
collected  extractive  called  the  p ercolate.

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• Most drug extractions are performed by percolation .

• In the process of percolation the flow of the menstruum over

the drug column is generally downward to the exit orifice,
drawn by the force of gravity as well as the weight of the
column of liquid.

• In certain specialized and more sophisticated percolation

apparatus, additional pressure on the column is exerted with
positive air pressure at the inlet and suction at the outlet or exit.

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• Percolators for drug extraction vary greatly as to their shape,

capacities, composition, and, most important utility.

• Percolators employed in the large-­scale industrial

preparation of extractive are generally stainless steel or glass
lined metal vessels that vary greatly in size and in operation.

• Percolation on a small scale generally involves the use of

glass percolators of various shapes for extraction of small
amounts (perhaps up to 1000 g) of crude drug.

COLLEGE  OF   PHARMACY

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Different  shapes  of  percolator

1.  Cylindrical,  with  little,  if  any  taper  
except  for  the  lower  orifice  also  
called  Oldberg  percolator.
2.  roundish,    but  with  a  definite  taper  
downward.
3.  Conical  or  funnel  shape.
Ø The   cylindrical  percolator  i s  
particularly  suited  to  the  complete  
extraction  of  drugs  with  a  minimal  
expenditure  of  menstruum.

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• The  choice  o f  type  o f  Percolator  d epends  u pon

1. Nature of the drug
2. Type of product prepared
3. Quantity of drug to be extracted
• Processes  and  steps  o f  Percolation
1. Preparation of the dried crude drug for percolation
a. Powdering
b. Moistening
2. Packing the percolator
3. Period of Maceration
4. Percolation and collection of percolate
5. Adjustment of concentration of percolation as required
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Modifications
• In  general  process  of  percolation  the  following  problems  may  
arise:  
a)   If  the  active  substances  are  thermo-­labile,  evaporation  of  
large  volume  of  dilute  percolate,  may  result  in  partial  loss  of  the  
active  constituents.  
b)   In  the  case  of  alcohol-­ water  mixture,  evaporation  results  in  
preferential  vaporization  of  alcohol  leaving  behind  an  almost  
aqueous  concentrate  which  may  not  be  able  to  retain  the  
extracted  matter  in  solution  and  hence  get  precipitated.  
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Reserved  Percolation  
ØIn  this  case  the  extraction  is  done  through  the  general  
percolation  procedure.  
ØAt  the  last,  the  evaporation  is  done  under  reduced  
pressure  in  equipment  such  that  all  the  water  is  
removed.  
ØThis  is  then  dissolved  in  the  reserved  portion  which  is  
strongly  alcoholic  and  easily  dissolves  the  evaporated  
portion  with  any  precipitation  
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(3) Decoction
This method involve the placement of plant material in water, then boiling the mixture
for about 15 minute, followed by filtrations to obtain the extractive and removing the
marc.

(4) Digestion
Maceration with continued heating during maceration period. The temperature is
between 40 ℃– 60 ℃.

(5) Infusion
Involves first macerating the drug with cold water, followed by the addition of boiling
water in an amount equal to 90% of the desired volume.

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Thanks  for  your  attention  

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