M1 Evaluation of Crude Drugs: Introduction
Simple
Crude Drugs are defined as natural product usually of plant or
animal origin that only undergone the process of collection
and drying. This term is generally applied to plant or animal
products found in their raw form --- no man-made changes are
made in their molecular structure.
Evaluation of drug means confirmation of its identity and
determination of its quality and purity. The main reasons behind
the need for evaluation of crude drugs are biochemical
variation in the drug, effect on treatment and storage of
drugs, and the adulteration and substitutions.
This module focuses mainly on the physical and chemical as
well as organoleptic evaluation of some crude drugs.
The different ways in which crude drugs can be evaluated:
1. Organoleptic Evaluation
2. Microscopic Evaluation
3. Chemical Evaluation
4. Physical Evaluation
5. Biological Evaluation
Methods of Evaluation
ORGANOLEPTIC EVALUATION
Organoleptic evaluation means the study of drugs using organs
of senses. It refers to the methods of analysis like color, odor,
taste, size, shape and special features, such as touch, texture,
etc. Obviously, the initial sight of the plant or extract is so
specific that it tends to identify itself. If this is not enough,
perhaps the plant or extract has a characteristic odor or taste.
The study of form of a crude drug is morphology while
description of the form is MORPHOGRAPHY.
Examples:
 The fractured surfaces in cinchona, quillaia and cascara
barks and quassia wood are important characteristics.
 Aromatic odor of umbelliferous fruits and sweet taste of
liquorice.
 The wavy shape of rauwolfia, pungent taste of capsicum
and ginger, brown color of cinnamon, odor and taste of
spice-drugs like, asafoetida, black pepper, nutmeg,
caraway, cumin etc. are important diagnostic organoleptic
characteristics.
MICROSCOPIC EVALUATION 1.
This method allows more detailed examination of a drug and it 2. Rapid
can be used to identify the organised drugs by their known
3. Designed for a minimum of equipment
histological characters. It is mostly used for qualitative
evaluation of organised crude drugs in entire and powdered 4. Reasonably selective for the class of compounds under study
forms. Every plant possesses a characteristic tissue feature.
Microscope can be used to confirm the structural details of the 5. Quantitative in so far as having a knowledge of the lower limit
drugs from plant origin. For the effective results, various of detection is concerned; and if possible
reagents or stains can be used to distinguish cellular structure.
6. Should give additional information as to the presence or
CHEMICAL EVALUATION absence of specific members of the group being evaluated
The chemical evaluation includes qualitative chemical tests,
STEPS INVOLVED IN PHYTOCHEMICAL INVESTIGATION
quantitative chemical tests, chemical assays and instrumental
analysis. The isolation, purification and identification of active 1. Authentication and extraction
constituents are chemical methods of evaluation. 2. Separation and isolation of constituent of interest
3. Characterization of the isolated compound
Qualitative chemical tests include identification tests for various
4. Investigation of the biosynthetic pathway
phytoconstituents like alkaloids, glycosides, tannins,etc.
5. Qualitative evalutaion
6. Pharmacologic evaluation of the separated compound
PHYSICAL EVALUATION
Physical standards are to be determined for the drugs, wherever
COLLECTION (PLANTS)
possible. These are rarely constant for crude drugs, but may
help in evaluation, specifically with reference to moisture
content, specific gravity, density, optical rotation, refractive The proper time in the collection of plant parts for phytochemical
index, melting point, viscosity, and solubility in different solvents. screening is an important matter to consider. The plant part is
best collected as follows:
BIOLOGICAL EVALUATION
BEST TIME OF
 When the estimation of potency of crude drug or its preparation PART EXAMPLES
COLLECTION
is done by means of its effect on living organisms like bacteria,
fungal growth or animal tissue or entire animal, it is known After vegetative
Tubers, Bulbs,
as bioassay. This method is generally called for, when Roots or Rhizomes processed are
Ginger
standardization is not adequately done by chemical or physical ceased
means and also for conformity of therapeutic activity of raw
material and finished product. In other words, bioassay is the Before vegetative
process/ After the
measure of sample being tested capable of producing biological Stem or Bark Gugo, Cinchona,
effect as that of the standard preparation. Such activity is period of damp
represented in units known as international unit (I.U.) weather
When they are
The Phytochemical Investigation Flowers Sampaguita, Rose
about to bloom
Phytochemical investigation refers to the extraction, When they are fully
Seeds Pumpkin, Sunflower
screening and identification of medicinally active substances matured
found in plants. Different methods can be conducted to When
determine the different constituents present in plants. One of the Leaves photosynthesis is Ikmo, etc.
methods of identifying the constituents is through phytochemical active
screening.   
Fruits Unripe/Ripe Mango, Banana, etc.
Characteristics:
A method for use in phytochemical screening should be:
Extraction of Plant Material

Extraction depends on the nature of the plant material and the

components to be isolated. Dried materials should be powdered
before a. Fresh materials can be homogenized or soaked to a
solvent such as alcohol. Alcohol general solvent for extraction,
light petroleum (essential, fixed oils, steroids), ether and
chloroform (Alkaloids), water immiscible solvent (Alkaloids), and
acidification (aromatic acids & phenols).

M1 Exercise 2 Moisture Content
Moisture can be simply defined as water diffused in a relatively
minute quantity. Moisture content is relatively difficult to
accurately measure due to the complex intermolecular bonding
properties within the substance matrix. This property is an
important factor to identify among crude drugs mainly because
the moisture is largely responsible for the decomposition of
crude drugs through chemical change, microbial or fungal
growth.
Moreover, the presence of moisture may increase the following
physical properties of crude drugs: weight, density, viscosity,
refractive index and electrical conductivity. Therefore, the
moisture content determination is a crucial component of quality
of crude drugs and essentially a quality control parameter in
most production and laboratory facilities.
According to USP/NF, there are official two types of water
present in drugs: water of crystallization which is a definite
proportion of water as part of drug’s crystalline structure, and
water in the adsorbed form which is the water present in the
surface (whether internal or external) of the drug.
Moisture content can be determined through the following
official methods:
THERMOGRAVIMETRIC ANALYSIS
 This method involves the use of heating through convection
with forced or circulating hot air on the crude drug.
 The moisture content is the computed based on the loss of
mass of the substance on drying through water vaporization
after it was heated.
 The sample is weighed before and after the drying process
and the moisture content is computed on percentage basis.
There are two methods available utilizing this principle:
(a) Drying oven and balance method
The drying oven and balance method is the official reference
method for some substances and is used for cross-referencing
alternative methods. This method is useful for
very heterogenous large sample size (e.g. 500 g)
Disadvantage: time consuming compared to alternative
methods.
(b) IR moisture analyzer
The IR moisture analyzer is highly convenient for fast and
reliable moisture content analysis to avoid lengthy delays. This
method has a simple process and minimal errors due to
automatic calculated results.
VOLUMETRIC ANALYSIS
 This method involves the use of azeotropic distillation
principle wherein the liquid mixture is separated into pure
components with the help of an additional solvent known
as entrainer (e.g. toluene).
 This is usually applied for crude drugs with or without
volatile substances. During the process, the crude drug with
water, after the azeotrope is formed, is added with toluene
to separate the water and the organic components. The
water collected will be then directly measured through its
volume (mL or L).
TITRIMETRIC ANALYSIS
 also known as Karl Fischer titration, utilizes the quantitative
reaction of water with iodine and sulfur dioxide in the
presence of a low molecular weight alcohol (e.g. methanol)
and an organic base (e.g. pyridine). Mnemonics (P-I-M-S).
 During the process, once all the water present in the crude
drug is consumed, the presence of excess iodine is
determined volumetrically by the indicator electrode of the
titrator. The amount of water present in the sample is
calculated based on the concentration of the excess iodine.
There are two methods of KF titration:
(1) Volumetric KF titration determines moisture content by
measuring the amount of iodine consumed as a result of
reaction with water within the sample
(2) Colometric KF titration determines the moisture content by
measuring the quantity of electricity which is required for the
electrolysis.
M1 Exercise 3 Ash Content Determination of Crude Drugs
When vegetable drugs are incinerated, they leave an inorganic
ash which in the case of many drugs (e.g. rhubarb) varies within
fairly wide limits therefore making  little value for purposes of
evaluation.
Ash values are helpful to determine the quality as well as purity
of a crude drug, especially when the drug is present in
powdered form. The object of ashing crude drugs is to remove
the traces of organic matter which may be interferes in an
analytical determination.
ASH and ASH CONTENT DETERMINATION
Ash refers to the inorganic residue left after the moisture and
other organic substances had been removed by incinerating the
sample in the presence of oxidizing agents.
Ash content determination is one of the most widely employed
quality control parameter, based on fact that minerals are not
destroyed by heating.
This analytical test provides a measure of the total amount of
minerals in a sample, furnishes a basis for judging the identity
and purity of a drug and gives relative information on
adulteration with inorganic matter.
TOTAL ASH CONTENT
The total ash content refers to the residue remaining on the
vessel after the incineration. This allows to easily identify the
physiological and non-physiological materials contained in the
drug.
Physiological ashes are derived from the plant tissue itself while
non-physiological ashes are often derived from environmental
contamination (e.g. sand, soil). The total ash usually contains
carbonates, phosphates, sulfates, chlorides, oxides of calcium,
magnesium, potassium, sodium, aluminum, iron and other
metals. White heat 1200 to 1600°C

ACID - INSOLUBLE ASH

Another index to measure the purity and quality of plant samples

is the acid-insoluble ash. This ash refers to the part of the total
ash that is insoluble in dilute inorganic acids. The diluted
hydrochloric acid, for example, can dissolve calcium carbonate,
alkali chlorides, and the like, leaving an acid-insoluble residue
that consists almost entirely of silica from soil adhering to the
drug.
ASH CONTENT DETERMINATION - METHODS
IMPORTANT REMINDERS:
In doing the procedure, it is important to note that before using
the crucible, it is necessary to ignite it first to dull redness until
its weight is constant. This would remove any moisture and
adsorbed gases trapped or adhering into the crucible which can
affect the accuracy of the results. Moreover, the drug sample
must be incinerated at temperature not more than dull redness.

(1) Direct incineration of the sample placed in the crucible

using open flame burner:
The sample is placed in a crucible and cover and is incinerated
over an open flame burner set-up using a clay triangle, tripod
and a Bunsen burner. A crucible and cover can be made of a
porcelain or a more sophisticated quartz used for high-
temperature requirements up to 1050°C.
(2) Use a muffle furnace:
The working principle of this equipment is to heat the air inside
the chamber by heating a Nichrome (nickel-chromium) wires.
More often, a simple fan-based exhaust system supported by a
chimney operates to cool the unit.
This simple exhaust system takes out toxic gases inside the
chamber which comes out during the heating of the sample. The
temperature inside the furnace can be controlled and adjusted
using an electronic controller unit. The following are the
approximate temperatures used in incinerating the samples
inside the muffle furnace:
ASH CONTENT FORMULA
In doing the procedure, it is important to note that before using
the crucible, it is necessary to ignite it first to dull redness until
its weight is constant. This would remove any moisture and
adsorbed gases trapped or adhering into the crucible which can
affect the accuracy of the results. Moreover, the drug sample
must be incinerated at temperature not more than dull redness.
In this exercise, muffle furnace will be employed in measuring
the ash content of the crude sample. Moreover, the acid-
insoluble ash will also be computed based from the obtained
total ash. The total ash and acid-insoluble ash will be computed
using the formula indicated below, respectively:

Heating description Temperature

Very dull red heat 500 to 550°C

Dull red heat 550 to 700°C

Bright red heat 800 to 1000°C

Yellow red heat 1000 to 1200°C