Pharmaceutical Analysis

1. WELCOMES YOU

2. Presented by:-
Meraj Khan
M pharma (Pharmacology)

3. Definition
Pharmaceutical analysis is a branch of practical chemistry that
involves a series of process for identification, determination,
quantification and purification of a substance, separation of
the components of a solution or mixture, or determination of
structure of chemical compounds.
The substance may be a single compound or a mixture of
compounds and it may be in any of the dosage form.
The substance used as pharmaceuticals are animals, plants,
micro organisms, minerals and various synthetic products.

4. BASIC OF ANALYSIS
Assay:- is an investigative (analytic) procedure in Laboratory
for qualitatively assessing or quantitatively measuring the
presence, amount, or functional activity of a target entity (the
analyte).
Analyte:- It is the chemical entity under assay e.g., HCl.
Titrant:- It is the solution of known strength (or
concentration) employed in the assay e.g., NaOH.
Titration:- is the process of adding and then actually
measuring the volume of titrant consumed in the assay.
This volume is usually measured by the help of a calibrated
burette.

5. Indicator:- is a chemical substance sensitive enough to display an
apparent change in colour very close to the point in the ongoing
titration process at which equivalent quantities of analyte and
titrant. E.g. Methylene blue
Equivalence Point (or Stoichiometric Point):- is the point at
which one species neutralize the opposite species or is visibly
spotted by the use of indicators.
example The point at which Acid neutralize the base is
Equivalence Point.
End point :- The point at which color start to change during
titration process.
Titration Error:- Difference between end pont and equivalent
point is called Titration Error.

6. Analyse:-The sample to be analysed is called as analyse.
Standardization is the actual determination of either the
normality or the molarity of a solution.
Primary Standard is the substance of known purity (‘AnalaR’-
grade reagents) whose carefully weighed quantity helps in the
standardization of an unknown solution.Eg. Na2CO3
Secondary Standard is another standard solution that is used for
standardization of an unknown solution. eg:- NaOH
Titer is the weight of a substance chemically equivalent to 1 ml of a
standard solution.
Example : 1 ml of 1 N HCl contains 0.03646 g of HCl and hence is
chemically equivalent to 0.04000 g of NaOH.

7. TYPES OF ANALYSIS
There are main two types of chemical analysis.
1. Qualitative (identification)
2. Quantitative (estimation)
1. Qualitative analysis:-
It 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, colour change reactions, melting point
and boiling point test etc.

8. 2. Quantitative analytical:-
These techniques are mainly used to quantify any compound
or substance in the sample.
These techniques are based in:-
The quantitative performance of suitable chemical reaction
and either measuring the amount of reagent added to
complete the reaction or measuring the amount of reaction
product obtained
The charatristic movement of a substance through a defined
medium under controlled conditions.
Electrical measurement
Measurement of some spectroscopic properties of the
compound.

9. ON THE BASIS OF SIZE OF SAMPLE, THEY CAN BE
CLASSIFIED AS :-
I. Macro(0.1 g or more)
II. Semi micro (0.01 g to 0.1 g)
III. Micro(0.001 g to 0.01 g)
IV. Sub micro (0.0001 g to 0.001 g)
V. Ultramicro (below 10-4 g)
VI. Trace analysis(100 to 10000 ppm).
Among all, the semi micro analysis is widely used.

10. METHODS OF
ANALYSIS
I
INSTRUMENTAL
NON-INSTRUMENTAL
Electro Analytical
Spectro
Analytical
Chromatography
Other techniques
Biological
methods
Chemical
methods
Electro -
gravimetry
Conducto -
metry
Coulometry
Potentiometry
Voltametry
Spectrophotometry
Spectrofluromtry
IR
Spectrophotom
etry
Atomic emission
spectroscopy
Atomic absorption
spectroscopy
Flame emission
spectroscopy
Turbidimetry
Nephelometry
Colorimetry
Ion pair
extraction
Colour development by
chromogen
GLC
HPLC
TLC/HPTLC
RIA
Flow
injection
ELISA
Animal assay
Microbiological
Assay
Titrimetry Gravinmetry
Acid
base
Redox
Precipitation
Complexo etry
Non aqueous

11. 1.CHEMICAL METHODS
a) 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.
There are Various types of Titrimetric methods are:-
i)Acid-base titrations (Aqueous titrations /Neutralization
reactions)
ii)Non aqueous titrations
iii)Redox Methods:-
Iodimetric Titrations
Iodometric Titrations
iv) Precipitation titrations
v)Oxidation reduction titrations
vi)Complexometric titrations

12. b) 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.
Advance method:-
Thermogravimetry Analysis (TGA):- records the change in
weight.
Differential Thermal Analysis (DTA):- records the difference
in temperature between test substance and an inert reference
material
Differential Scanning Calorimetry (DSC):- records the energy
needed to establish a zero temperature difference between a test
substance and reference material.

13.  c) Gasometric Analysis:-
Gasometry involves measurement of the volume of gas
evolved or absorbed in a chemical reaction. Some of
the gases which are analysed by Gasometry are CO2 ,
N2O,cyclopropane, amyl nitrate, ethylene, N2, helium
etc.

14. 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:-
(a)Potentiometry:- It measures electrical potential of an
electrode in equilibrium with an ion to be
determined.example.PH meter.
(b)Conductometry:- It measures electrical conductivity of an
electrode with a reference electrode.
(c) Voltametry:- It measures electrical current at a micro-
electrode. example:- Polarography, Amperometry

15. 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.

16. 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 ultra
violet, 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.

17. Chromatographic techniques and electrophoretic
methods are separation methods for the mixure of
compounds, but also applied for identification of compounds
of mixures.
Various chromatographic techniques are GC, HPLC, TLC,
HPTLC, PC etc.
Mass spectrometry involves vaporization of material using a
high vaccum 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.

18. 4. BIOLOGICAL AND
MICROBIOLOGICAL METHODS
Biological methods are used when potency of a drug or its
derivative can not be properly determined by any physical or
chemical methods.
They are measured by 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 turbidimetric
analysis.

19. APPLICATIONS:-
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.
Determination of radioactive compounds.
Determination of natural phytoconstituents.
Determination of moisture or water contain of sample by using
Karl fischer titration.
Quantitative estimation of Nitrogen by using Kjeldahls
Mrthod.

20. THANK YOU