Department of Pharmaceutical Chemistry

511-P Pharmaceutical Chemistry-IIIA (Pharmaceutical Analysis)

Date:
INTRODUCTION TO PHARMACEUTICAL ANALYSIS
Pharmaceutical analysis is a broader term which can be defined in many ways. It is the series
of processes that are used for identification, determination, separation, purification, and
structure elucidation of the given compound used in the formulation of pharmaceutical
products. The components, to which the pharmaceutical analysis is done, are normally active
pharmaceutical ingredients, pharmaceutical excipients, contaminants present in
pharmaceutical products, or drug metabolites. In pharmaceutical analysis, the samples are
typically finished pharmaceutical products, biological samples, impurities, contaminants, and
pharmaceutical raw materials. Pharmaceutical analysis can be done using various analytical
techniques. This is mainly used for the separation of the components from the mixture and for
the determination of the structure of the compounds. The different pharmaceutical agents are
as follows:
 Plants
 Microorganisms
 Minerals
 Synthetic compounds

The substance maybe a single compound or a mixture of compounds and it maybe in any of
the dosage form. The substance used as pharmaceuticals are animals, plants, microorganisms,
minerals and various synthetic products.
The sample to be analyzed is called as analyte and on the basis of size of sample, they can be
classified as macro (0.1gormore), semi micro (0.01gto0.1g), micro (0.001gto0.01g), sub
micro (0.0001 g to 0.001 g), ultra-micro (below 10-4 g), trace analysis (100 to 10000 ppm).
Among all, the semi micro analysis is widely used.
 TYPES OF PHARMACEUTICAL ANALYSIS:
Based upon the determination type, there are mainly two types of analytical methods. They
are as follows:
1. Qualitative (identification)
2. Quantitative (estimation)
1. Qualitative analysis:
It is performed to establish composition of natural/synthetic substances. These tests are
performed to indicate whether the substance or compound is present in the sample or not.
Various qualitative tests are detection of evolved gas, formation of precipitates, limit tests,
color change reactions, melting point and boiling point test etc.
2. Quantitative analytical techniques:
They are mainly used to quantify any compound or substance in the sample. These
techniques are based on:
a) The quantitative performance of suitable chemical reaction and either measuring the
amount of reagent added to complete their action or measuring the amount of reaction
product obtained
b) The characteristic movement of a substance through a defined medium under
controlled conditions
c) Electrical measurement
d) Measurement of some spectroscopic properties of the compound.

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 Department of Pharmaceutical Chemistry
511-P Pharmaceutical Chemistry-IIIA (Pharmaceutical Analysis)
Date:
VARIOUS SUB-CLASSIFICATION OF QUALITATIVE ANALYSIS:
1. Chemical methods
 Volumetric or titrimetric methods
 Gravimetric methods
 Gasometric analysis
2. Electrical methods
3. Instrumental methods
4. Biological and microbiological
1. Chemical Methods:
 Titrimetric or volumetric method
It involves reaction of substance to be determined with an appropriate reagent as a standard
solution, and volume of solution required to complete the reaction is determined. Volumetric
methods require simple and less apparatus and they are susceptible of high accuracy.
Various types of titrimetric methods are:
a) Acid-base titrations (neutralization reactions)
b) Complexometric titrations
c) Precipitation titrations
d) Oxidation reduction titrations
e) Non aqueous titrations
 Gravimetric methods:
In gravimetric analysis, a substance to be determined is converted into an insoluble
precipitate in the purest form, which is then collected and weighed. It is the time consuming
process.
In electrogravimetry (EG), electrolysis of the sample is carried out on the electrodes is
weighed after drying. Thermogravimetry (TG) records the change in weight, differential
thermal analysis (DTA) records the difference in temperature between test substance and an
inert reference material, differentials canning calorimetry (DSC) records the energy needed to
establish a zero temperature difference between a test substance and reference material.
 Gasometric analysis:
Gasometry involves measurement of the volume of gas evolved or absorbed in a chemical
reaction.
Some of the gaseswhich are analyzed by Gasometry are CO2, N2O, cyclopropane, amyl
nitrate, ethylene, N2, helium etc.
2. Electrical Methods:
Electrical methods of analysis involve the measurement of electric current, voltage or
resistance in relation to the concentration of some species in the solution.
Electrical methods of analysis include:
 Potentiometry
 Conductometry
 Polarography
 Voltametry
 Amperometry
Potentiometry measures electrical potential of an electrode in equilibrium with an ion to be
determined. Conductometry measures electrical conductivity of an electrode with a reference
electrode while Polarography, Voltametry and Amperometry measures electrical current at a
micro-electrode.

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 Department of Pharmaceutical Chemistry
511-P Pharmaceutical Chemistry-IIIA (Pharmaceutical Analysis)
Date:
3. Instrumental Methods of Analysis:
Instrumental method involves measurement of some physical properties of the compound or a
substance. These methods are employed for determination of minor or trace concentration of
element in the sample.
Instrumental methods are preferred due to their selectivity, high speed, accuracy and
simplicity of analysis. Any change in the properties of the system are detected by
measurement of absorbance, specific rotation, refractive index, migration difference, charge
to mass ratio etc.
Spectroscopic methods of analysis depend upon measurement of the amount of radiant
energy of a particular wavelength emitted by the sample.
Methods which include absorption of radiation are ultraviolet, visible, infra-red, atomic
absorption, nuclear magnetic resonance spectroscopy etc.
Emission methods involve heating or electrical treatment of the sample so that the atoms are
raised to the excited state to emit the energy and the intensity of this energy is measured.
Emission methods include emission spectroscopy, flame photometry, flourimetry etc.
Chromatographic techniques and electrophoretic methods are separation methods for the
mixture of compounds, but also applied for identification of compounds of mixtures. Various
chromatographic techniques are GC, HPLC, TLC, HPTLC, PC etc.
Mass spectrometry involves vaporization of material using a high vacuum and the vapour is
bombarded by a high energy electron beam. Vapour molecules undergo fragmentation to
produce ions of varying size. These ions are differentiated by accelerating them in electrical
field and then deflecting them in a magnetic field. Each kind of ion gives a peak in the mass
spectrum.
4. Biological and microbiological methods:
Biological methods are used when potency of a drug or its derivative cannot be properly
determined by any physical or chemical methods. They are called bio-assays.
Microbiological methods are used to observe potency of antibiotic or anti- microbial agents.
In antimicrobial assay, inhibition of growth of bacteria of the sample is compared with that of
the standard antibiotic. These methods include cup plate method and turbid metric analysis.
 APPLICATIONS OF PHARMACEUTICAL ANALYSIS:
Manufacturing industries require both qualitative and quantitative analysis to ensure that their
raw materials meet certain specifications, and to check the quality of final product. Raw
materials are to be checked to ensure that the essential components are present within the
predetermined range of composition and there are not any unusual substances present which
might upset the manufacturing process or it may appear as a harmful impurity in the final
product.
In the development of new products which contains mixtures other than the pure material, it
is necessary to ascertain composition of mixture which shows the optimum characteristics
for which the material has been developed.
Geographical surveys require analysis to determine the composition of soil sample and
numerous rock samples collected from the field.
Most of the industrial processes give rise to pollutants which may cause health related
problems. So quantitative analysis of air, water and soil sample should be carried out to
determine the level of pollution and to establish the safe limits for pollutants

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