PRESENTED BY : PRIYANKA M. YADAV
M.PHARM (QA) SEM - 3
GUIDED BY : Mrs. NISHA H.
DEPARTMENT OF QUALITY ASSUARANCE
ARIHANT SCHOOL OF PHARMACY
HERBAL DRUGS/ HERBAL FORMULATION
• ARE – Finished labelled products that contain active
ingredients such as aerial or underground parts of plant or
other plant material or combinations thereof, whether in the
crude state or as plant preparations.
• ARE - crude plant material such as leaves, flowers, fruit, seed,
stems, wood, bark, roots, rhizomes or other plant parts, which may
be entire, fragmented or powdered.
Phytomedicines or Phytopharmaceuticals sold as Over The
Counter ( OTC ) products in modern dosage forms such as
Tablets, Capsules & Liquids for oral use.
Dietary Suppliments containing Herbal Products, also called
Neutraceuticals available in modern dosage forms.
Herbal Medicines consisting of either Crude, Semi Processed
or Processed Medicinal Plants.
Gums, Resins & Dyes
India’s strength in Herbal Technology
a l C o m m u n i t ie s ( o r a l)
India’s strength in Herbal Technology
Guidelines for Quality Control
of Herbal formulation
• Quality control of crude drugs material, plant preparations
and finished products
• Stability assessment and shelf life
• Safety assessment; documentation of safety based on
experience or toxicological studies
• Assessment of efficacy by pharmacological informations
and biological activity evaluations
• Standardization of drug means
“confirmation of its identity and
determination of its quality and purity and detection of
nature of adulterant by various parameters like
morphological, microscopical, physical, chemical and
OF HERBAL DRUGSOF HERBAL DRUGS
• Moist. Cont.
• Extrac. Values
• Ash Values
• Fluores. Analy.
• SEM Studies
• Powder Studies
A) Total viable
Determination of heavy
• Radioactive contamination
HPTLC Finger printing
DNA Finger printing
Standardization & Quality Evaluation of
• Visual inspection provides the
simplest and quickest means by
which to establish identity,
purity and quality.
• Macroscopic identity of
medicinal plant materials is
based on shape, size, colour,
surface characteristics, texture,
fracture characteristics and
appearance of the cut surface.
• Detail of cell structure and arrangement of the
cells useful for differentiating similar species.
• Select a representative sample of the material & If it is
dried parts of a plant than it may require softening before
preparation for microscopy, preferably by being placed in
a moist atmosphere, or by soaking in water.
• Any water-soluble contents can be removed from the cells
by soaking in water. Starch grains can be gelatinized by
heating in water.
• Measurement of specimen
• Stomatal number
• Stomatal index
• Palisade ratio
• Vein-islet number
• Vein termination number
• Lycopodium spore method
Foreign organic matter
• Parts of the medicinal plant material or
materials other than those named with the
limits specified for the plant material
• Any organism, part or product of an
organism, other than that named in the
specification and description of the plant
• Mineral admixtures that is adhering to the
medicinal plant materials, such as soil, stones,
sand, and dust.
Foreign matter: NMT 2%w/w
• It involves non-volatile inorganic components.
• High ash value is the indicative of contamination, substitution,
adulteration or carelessness in preparing the crude drugs.
• Total ash is designed to measure the total amount of material
produced after complete incineration of the drug material at as
low temperature as possible (about 450°C) to remove all the
• Total ash usually consists of carbonates, phosphates, silicates
• IP and USP: 675±25°C
• BP : 600±25°C
• WHO: 500-600°C
Acid insoluble ash
• Ash insoluble in HCl is the residue obtained after
extracting the total ash with HCl. It gives idea about the
• IP method: 25mL 2M HCL solution
• USP method: 25mL 3N HCL solution
• BP method: 15mLwater and 10mL HCL
• WHO method: 25 ml of hydrochloric acid (~70g/l)
Water soluble ash
• Total ash content which is soluble in water. It’s good
indicator of presence of previous extraction of water soluble
salts in the drug or incorrect preparation or amount of inorg.
• Carbonated ash: Ash is treated with ammonium carbonate.
• Nitrated ash: Ash is treated with dilute nitric acid.
• Amount of the active constituents present in crude drug
material when extracted with specific solvent.
• There are following
Methods for determin-
-nation of Extractive
a) Cold method
b) Hot method
• Presence of woody matter or vegetable debris or pieces of
• Eg. In catechu
Water insoluble matter: NMT 33%
Alcohol insoluble matter: NMT 30%
Total solid content
• The residue obtained when prescribed amount of preparation
is dried to constant weight under the specified condition
(Residue on evaporation)
• Powdered extract: NLT 95%
• Semisolid extract: NLT 70%
• Loss on drying (Gravimetric determination)
• Volumetric Azeotropic distillation (toluene distillation)
• Titrimetric Karl fisher method
• Gas chromatographic method
Volatile oil content
• Volatile oils are the liquid components of the plant cells,
immiscible with water, volatile at ordinary temperature and
can be steam distilled at ordinary pressure
• Many herbal drugs contain volatile oil which is used as
• E.g. Clove: NLT 15%v/w
• Medicinal plant materials that have a strong bitter taste
("bitters") are employed therapeutically, mostly as appetizing
agents. Their bitterness stimulates secretions in the
gastrointestinal tract, especially of gastric juice.
• The bitter properties of plant material are determined by
comparing the threshold bitter concentration of an extract of
the materials with that of a dilute solution of quinine
• The bitterness value is expressed in units equivalent to the
bitterness of a solution containing 1g of quinine hydrochloride
R in 2000 ml.
• Bitterness value calculated in units per g using the
a= the concentration of the stock test solution (ST) (mg/ml),
b = the volume of test solution ST (in ml) in the tube with the
threshold bitter concentration,
c = the volume of quinine hydrochloride R (in mg) in the tube
with the threshold bitter concentration.
• Many medicinal plant materials, of the families
Caryophyllaceae, Araliaceae, Sapindaceae, Primulaceae,
and Dioscoreaceae contain saponins.
• The most characteristic property of saponins is their
ability to cause haemolysis; when added to a suspension
of blood, saponins produce changes in erythrocyte
membranes, causing haemoglobin to diffuse into the
• The haemolytic activity of plant materials, or a
preparation containing saponins, is determined by
comparison with that of a reference material, saponin R,
which has a haemolytic activity of 1000 units per g.
• Calculate the haemolytic activity of the medicinal plant
material using the following formula:
1000 = the defined haemolytic activity of saponin R in relation to ox
a = quantity of saponin R that produces total haemolysis (g)
b = quantity of plant material that produces total haemolysis (g)
Determination of tannins
• Tannins (or tanning substances) are
substances capable of turning animal hides
into leather by binding proteins to form
water-insoluble substances that are resistant
to proteolytic enzymes.
• This process, when applied to living tissue,
is known as an "astringent" action and is
the reason for the therapeutic application of
• Chemically, tannins are complex
substances; usually occur as mixtures of
polyphenols that are difficult to separate and
• Calculate the quantity of tannins as a percentage using the
where w = the weight of the plant material in grams
T1= Weight of material extracted in water
T2= Weight of material not bound to hide powder
T0= Weight of hide powder material soluble in water
Determination of swelling
• The swelling index is the volume in ml taken up by the
swelling of 1 g of plant material under specified
• Its determination is based on the addition of water or a
swelling agent as specified in the test procedure for each
individual plant material (either whole, cut or pulverized).
Determination of foaming
• Many medicinal plant materials contain saponins that can
cause a persistent foam when an aqueous decoction is shaken.
• The foaming ability of an aqueous decoction of plant materials
and their extracts is measured in terms of a foaming index.
Calculate the foaming index using the following formula:
where a = the volume in ml of the decoction used for
preparing the dilution in the tube where foaming to a
height of 1 cm is observed.
foaming index =
Determination of pesticide
• Not more than 1%
• An ARL (in mg of pesticide per kg of plant material) can be
calculated on the basis of the maximum acceptable daily intake
of the pesticide for humans (ADI), as, recommended WHO,
and the mean daily intake (MDI) of the medicinal plant
ADI = maximum acceptable daily intake of pesticide (mg/kg of body weight);
E = extraction factor, which determines the transition rate of the pesticide from
the plant material into the dosage form;
MDI = mean daily intake of medicinal plant product.
Some example of Pesticides :
• Chlorinated hydrocarbons and related pesticides: BHC, DDT
• Chlorinated phenoxyalkanoic acid herbicides: 2,4-D; 2,4,5-T
• Organophosphorus pesticides: malathion, methyl parathion, parathion
• Carbamate insecticides: carbaryl (carbaril)
• Dithiocarbamate fungicides: ferbam, maneb, nabam, thiram, zineb
• Inorganic pesticides: calcium arsenate, lead arsenate
• Miscellaneous: ethylene dibromide, ethylene oxide, methyl bromide
• Pesticides of plant origin: tobacco leaf and nicotine; pyrethrum flower,
pyrethrum extract and pyrethroids; derris root and rotenoids.
Determination of arsenic and
• Contamination of medicinal plant materials with arsenic
and heavy metals can be attributed to many causes
including environmental pollution and traces of pesticides.
• Limit test for arsenic
• Limit test for cadmium and lead
• The contents of lead and cadmium may be determined by
inverse voltametry or by atomic emission
• The following maximum amounts in dried plant materials,
which are based on the ADI values, are proposed:
▫ lead, 10 mg/kg;
▫ cadmium, 0.3 mg/kg.
Test strains and culture media for use in validating the
tests for specific microorganisms
Table 1. Limits for microbial contaminants in finished products & Raw materials
• Aflatoxins are naturally occuring mycotoxins produced
mainly by Aspergillus flavus and Aspergillus parasiticus.
• The presence of aflatoxins can be determined by
chromatographic methods using standard aflatoxins B1,
B2, G1, G2 mixtures.
• IP method: NMT 2 µg/kg of aflatoxins B1& Total aflatoxins 4 µg/kg
• USP method: NMT 5ppb of aflatoxins B1& Total aflatoxins 20ppb
• The range of radionuclides that may be released into the
environment as the result of a nuclear accident might include
long-lived and short-lived fission products, actinides, and
• Microbial growth in herbals is usually avoided by irradiation.
This process may sterilize the plant material but the
radioactivity hazard should be taken into account.
• The nature and the intensity of radionuclides released may
differ markedly and depend on the source (reactor,
reprocessing plant, fuel fabrication plant, isotope production
• The radioactivity of the plant samples should be checked
accordingly to the guidelines of International Atomic
CHROMATOGRAPHY OF HERBAL DRUG
• Seperation, identification,
impurity detection and assay
of herbal drug in the
formulation or in the extract
are carried out by following
a) T.L.C. Finger-print profile of Methanolic extract of
(a) Under UV 366nm (b) Under UV 254 nm. (c) Under visible light after
b) Comparative HPTLC profile of Berberine in different
c) Densitometric scan of different samples
of Berberis spp. at UV 266 nm
ANALYTICAL SPECIFICATIONS OF VATI/GUTIKA
2. Weight variation
3. Disintegration time -Not more than 15 min
4. Identification TLC/HPTLC/GLC
6. Test for heavy/Toxic metals
7. Microbial contamination
Total bacterial count
Total fungal count
8. Test for specific Pathogen
9. Pesticide residue
11 Test for Aflatoxins (B1,B2,G1,G2)
ANALYTICAL SPECIFICATIONS OF
SYRUP (LIQUID ORAL)
1. Description, Colour
3. Total – ash
4. Acid – insoluble ash
5. Water-soluble extractive
6. Alcohol – soluble extractive
8. Total sugar content
10. Identification TLC/HPTLC/HPLC
11. Test for heavy metals
12. Microbial contamination
Total bacterial count
Total fungal count
13. Test for specific Pathogen
14. Pesticide residue
ANALYTICAL SPECIFICATIONS OF ASAVA
1. Specific gravity at 250 C.
2. Alcohol content
Test for methanol.
3. Total acidity.
4. Non reducing and reducing sugar.
Other specifications same as oral
ANALYTICAL SPECIFICATIONS OF
(FINE POWDER)/KVATHA CURNA
(COARSE POWDER FOR DECOCTION)
1. Loss on drying at 105 ºC
2. Particle size (80-100 mesh for Churna;
40-60 mesh for Kvatha churna)
Other specifications are same as
Parameter & its specifications
Total Bacterial count - 1 x 1055
Yeast & Mould - 1 x 103
E. coli - Absent
Salmonella - Absent
P. Aeruginosa - Absent
S. Aureus - Absent
2. Pesticide Residue – Less than 1 ppm
ACCEPTABLE LIMITS FOR
3. Heavy metals
Lead - 10 ppm
Mercury - 01 ppm
Arsenic - 03 ppm
Cadmium - 0.3 ppm
B1 - 0.5 ppm
G1 - 0.5 ppm
B2 - 0.1 ppm
G2 - 0.1 ppm
1. Kokate C.K., Gokhale, S.B. 2001. Practical Pharmacognosy. 2nd
ed. Nirali Prakashan,
Pune, p. 14-19.
2. Mukherjee P.K. 2010. Quality control of herbal drugs. 4th
ed. Business Horizones, New Delhi,
3. Ansari S.H. 2006. Essentials of Pharmacognosy. 1st
ed. Birla Publications, New Delhi, p. 581-
5. WHO guidelines ISBN 978 92 4 1547 16 1.
6. Anonymous, 2010. Indian Pharmacopoeia. Vol.-3, Government of India, Ministry of Health
and Family Welfare, New Delhi p. 2467-2472.