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Special Methods Used in Pharmaceutical Analysis

Crude drugs

 Plant exudates
 Products of collection and drying of natural substances
 Vegetable/ animal drugs consists of natural substances
 Qualitative analysis of crude drugs and of the products derived from them are
made to establish purity or to determine the amount of therapeutically active
constituents present for the purpose of standardization.

Classifications of Special Methods:

1. Chemical Methods

 Employed in the determination of ash, moisture, crude fiber, extractive obtained

with different solvents, the estimation of alkaloidal content, etc.
2. Biological Methods

 Methods which the effects of drugs upon microbes, animals or animal tissue are
 Employed in the absence of satisfactory chemical methods of standardization.
 Biological methods require special apparatus for their performance and a
technique that is not chemical in nature.

Ash and Water Determination

Ash Content

 The ash content of a crude drug is generally taken to be the residue remaining
after incineration.
 INCINERATION – an analytical procedure of heating an organic substance with
free access to air until only its ash remains.
 This usually represents the following:
o Inorganic salts naturally occurring in the drug and adhering to it
o Inorganic matter added for the purpose of adulteration
 ADULTERATION – admixtures or substitutions of original or genuine article/ drug
with inferior, defective or otherwise useless or harmful substances.
 Ash determination furnishes a basis for judging the identity and cleanliness of a
drug and gives information relative to its adulteration with organic matter.
 The ash (residue) yielded by an organic chemical compound is, as a rule, a
measure of the amount of inorganic matter present as Impurity.
 TOTAL ASH – residue remaining after incineration
 ACID-INSOLUBLE ASH – part of the total ash which is insoluble in diluted HCl
 The careful control of temperature is the most important analytical factor to
regulate in making ash determination.
 All determinations should be made in such a manner as to duplicate insofar as
possible the conditions under which standards are established.

Temperature Equivalents (Using electric furnace for ignition)

Very dull-red heat 500 – 550 °C

Dull-red heat 550 – 700 °C
Bright-red heat 800 – 1,000 °C
Yellow-red heat 1,000 – 1,200 °C
White heat 1,200 – 1,600 °C

Practically, all these temperatures are within the limits of the ordinary Bunsen
burner, depending on the construction of the burner and the nature of the gas burned.

Residue on Ignition

 The ash content of chemicals is determined by ignition to dull redness in the

same manner as in the determination of the ash content of a crude drug.
 It is economically impractical to make ash determinations on large samples of
expensive chemicals.
 However, it is necessary to control the amount of inorganic matter that may be
contained in such substances as alkaloidal salts, especially when the substance
is intended for hypodermic administration.
 Official standards (found in USP-NF) require that small amounts of expensive
substances be used, and that the ash yielded to be negligible.
 NEGLIGIBLE – quantity of ash not exceeding 500µg
Loss on Ignition (Loss on Drying)

 This technique provides a means of determining the percentage of test material

which is volatilized and driven off under the conditions specified.
 It is determined by heating the sample below its melting point in an oven and it
includes all volatile matter including water content and solvents.

Water Content (Moisture Content)

 Many drugs contain varying quantities of water, either as water of crystallization

(hydrates) or as water in the adsorbed form.
 When crude drugs are sold with a guaranteed assay for active constituent, the %
active constituent must be calculated on the basis of the moisture-free drug.

Methods of Water Content Determination

(1) Gravimetric Method for drugs containing no constituent, other than water, volatile
at 105 °C.
a. 10 grams of drug is accurately weighed and dried in an oven at 105°C for
5 hours. After 5 hours, the sample is weighed and again dried at 1-hour
intervals until the loss in weight is not more than 0.25% in 1-hour of drying.
b. The weight loss of the drug represents the moisture present in the sample.

(2) Gravimetric Method for drugs containing ether-soluble constituents, volatile at

a. The moisture content of the drug is determined by subtracting the weight
of ether-soluble extractive from the weight lost by the drug upon drying
b. Uses anhydrous ether for extraction

(3) Azeotropic Method (Toluene Distillation)

a. Employed for vegetable drugs containing 2% or more of moisture.
b. Disadvantage: a large amount of drug is required for the determination in
order to secure a volume of water that can be measured for the
conveniently without considerable error.

(4) Titrimetric Method (Karl Fischer Titration)

a. It is an accurate method of determining the amount of water
b. It is a chemical analysis procedure which is based on the oxidation of
sulfur dioxide by iodine in a methanolic hydroxide solution.
Karl Fischer Reagent:
Sulfur dioxide + iodine + pyridine (base) + methanol (solvent)

(5) Dew Point Method

(6) Electrolytic hygrometric Method