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Quality Control of Crude Drug

The document discusses quality control of crude drugs, which includes standardization and evaluation methods. Standardization determines quality, purity, potency, efficacy, and safety through organoleptic, microscopic, chemical, and other tests. Evaluation confirms identity through sampling and various analytical methods like organoleptic, microscopic, physical, chemical, and biological evaluations. Common quality control assays include ash values, extractive values, determination of active constituents by spectroscopy, chromatography, and other analytical techniques.

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Sudipta Saha
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612 views28 pages

Quality Control of Crude Drug

The document discusses quality control of crude drugs, which includes standardization and evaluation methods. Standardization determines quality, purity, potency, efficacy, and safety through organoleptic, microscopic, chemical, and other tests. Evaluation confirms identity through sampling and various analytical methods like organoleptic, microscopic, physical, chemical, and biological evaluations. Common quality control assays include ash values, extractive values, determination of active constituents by spectroscopy, chromatography, and other analytical techniques.

Uploaded by

Sudipta Saha
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Quality Control of Crude

Drug

Prof.(Dr.) U.S. Mishra


Dept.(P.A.&Q.A)
Quality Control
Quality control of crude drug mainly include
the standardization and evaluation method.
 Standardization means determination of
quality,purity,potency,efficacy andsafety
 Evaluation means confirmation of identity
 The synonym of quality control is assay of
active constituents followed by official
standards.
Standards of Identity&Purity
 Standards of Identity-These includes:-
 Organoleptic
 Microscopical/Histological character
 Deterioration of drug on storage
 Chemical tests
Standardization and Evaluation
Before a drug can be evaluated a sample must
be drawn for analysis.
 Sample is truely representative
 Different method of sampling is done from
large quantity of bulky drug
Methods of Evaluation
 Organoleptic Evaluation
 Microscopical Evaluation
 Physical Evaluation
 Chemical Evaluation
 Biological Evaluation
 Organoleptic Evaluation-It includes
colour,odour,taste,size,shape and surface
characteristic
 Microscopical Evaluation-It is important for
organized crude drug having definite cellular
structure
 Chemical Evaluation-This include chemical
tests
 Biological Evaluation
 Physical Evaluation:
1. It include-foreign analytical method,microbial
contamination,moisture content(loss on
drying,vaccum drying)
2. Ash values-Total ash values,Acid insoluble
ash,water soluble ash,sulphated ash
3. Extractive values-water soluble
extraction,ethanol extraction,pet.ether
extraction,ether extraction,volatile oil
determination
1. Physical parameter-M.P&B.P,R.I,Optical
rotation,Rf values
2. Spectroscopy method-UV,IR,NMR,MS,X-
RAY
3. Chromatographic method-
TLC,HPLC,HPTLC,GC
ASH VALUES
 Total ash-Place 2-4gm grounded material in a
crucible ↓
 Ignite it at 500-600ºc(until white)
 ↓
 Cool in a desicator and weigh it
 If carbon free ash can’t obtained,then cool the
residue with 2ml of water or saturated soln of
amm.nitrate
 ↓
 Dry on a waterbath,then on a hot plate
Ignite to constant weight
↓
Allow the residue to cool in a desicator(for
30mins)
↓
Weigh without delay & calculate the total ash
mg per gm
Acid Insoluble Ash
Total ash+25ml HCL cover with a watchglass
↓
Boil for 5 minutes
↓
Rinse the watchglass with 5ml hot water,add
liquid to the crucible
↓
Collect the insoluble matter on an ashless filter
paper&wash with hot water
↓
Transfer the insoluble matter to original
crucible
↓
Dry on hot plate & ignite to constant weight
↓
Cool the residue for 30 mins
↓
Weigh without delay,calculate the weight
Water Soluble Ash
Total ash+25ml of water
↓Boil for 5 min
Collect insoluble matter in a crucible on an ashless
filterpaper
↓wash with hot water
ignite for 5min at 450ºc
↓
Weight of total ash­weight of this residue
↓
Calculate content water soluble ash
Extractive Value
 This determines the amt. of active
constituents extracted with solvent
 Recommended Procedure-
 Method-1:Hot extraction-
4gm powdered drug +100ml water
↓weigh to obtain total
wt(flask)
Shake well,allow to stand for
1hour
↓
Attach reflux condenser to the flask
↓boil for 1hour,cool&weigh
Readjust to original total weight with solvent
↓shake well & filter it
Transfer 25ml of filtrate to tared flatbottomed disk

↓Evaporate to dry
Dry at 105ºc for 30min
↓cool in a desicator for 30min
Weigh& calculate the extractable matter
 Method-2:Cold Maceration-
4gm powdered material macerate with 100ml of solvent
for 6 hours
↓ shaking frequently
Allow to stand for 18 hours
↓ Filter it
Transfer 25ml to the tared flat bottomed disk
↓ Evaporate to dry
Dry at 105ºc for 6hours
↓cool it for 30min
Weigh & calculate the extracted matter
Determination of crude fibre
 Estimation of crude fibre denotes the
measurements of content of
cellulose,lignin,corkcells in plant tissue
 This is used for microscopic examination of
cellular materials(e.g.determine oleo-resin
&starch in ginger)
 It is also used for detection of presence of
adulterants
PROCEDURE
2gm of crude drug→Ether
extract+200ml1.25%H2So4(in 500ml)
↓Reflux for 30min
Filtration and residue washed with boiling water
↓until free from acid
Residue is rinsed back into flask with 200ml of
boiling 1.25%NaOH soln
↓boil for 30 min
Filter the liquid
↓
Residue on the filter is washed with boiling
water until neutral
↓
Dried at 110ºc to constant weight
↓
Incinerated to constant ant weight
 %of original wt of material ═ wt of dried
residue- wt.of incinerated residue
ASSAYS
 A crude drug may be assayed for a particular
group of constituents e.g. total alkaloids in
belladona or total glycosides of digitalis
 Biological assays is time-consuming and
applicable to those potent drugs
 The physical and chemical assays are
employed for routine standardization.
Types of assay employed for crude
drug
 Types of Assay  Examples
1. Separation & weighing  Colchicine from
of active constituents colchicum
 Total balsamic esters of
peru balsam
2. Chemical  Total alkaloid of many
drugs
 Strychnine from
nuxvomica
3. Physical
 Cineole in Eucalyptus
oil
 Spectrometric including  Most group of active
colorimetric & constituents
flouroscence
 Biological  Cardioactive
drugs,antibiotics,vitamin
s,antitumour drugs
 Radio Immuno Assay  Hespridin,morphine,trop
ane alkaloids,
vincristine
 Enzyme immuno assay
 Quassia,podophyllotoxi
ns
Spectroscopic Analysis
 The electromagnetic vibration utilized in
spectroscopic analysis
 This can be divided according to wavelength
into uv,visible,near IR & IR regions
 For this evaluation a substance of std. curve
is prepared by measuring the optical
densities
 The solution must be sufficiently diluted
Fluoroscence Analysis
 Many substances e.g.quinine in solution in
dilute sulphuric acid emit light of different
wavelength.
 For examination solids may be placed directly
under the lamp whereas liquid may be
examined in non-fluorocent dishes or test
tube or after spotting on filter paper
Quantitative fluoroscence analysis
 This tech. utilizes the fluoroscence produced
by a compound in uv light for quantitative
evaluation
 The instrument employed is a
fluorimeter,consists of uv source and
photoelectric cell to measure the intensity of
emitted light.
NMR
 This tech.is associated with structure
determination of organic compounds
 The use of H NMR has been described for
the assay of atropine and hyoscine in extract
of belladona,hyocyamus & stramonium
 IMMUNOASSAY- Used for quantitative
determination of compounds in biological
fluids.
RIA
 The assay depends on the specific reaction of
antigen and certain antibody
 Used in clincal analysis
 Example-Digitalis
ELISA-
Competition for an immobilized Ab takes place with a
modified form of the compound under
analysis(enzyme bounded)
↓
Release of compound-enzyme complex from binding
site(e.g.Alkaloid drugs)
Tandem mass spectroscopy(MS-MS)
 Mass spectroscopy is usually associated with
the structural elucidation of compounds
 By the two mass spectrometers it is possible
to determine quantitatively the amount of a
particular targeted compound incomplex
mixtures
e.g.used for analysis of cocaine in plant
material

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