BP102 T Pharmaceutical Analysis-

I Introduction to subject

Prepared By
Ram Kumar
Assistant Professor
DOPST
MRSPTU, Bathinda
Scope of the Subject

 This course deals with the fundamentals of analytical chemistry and

principles of electrochemical analysis of drugs.

2
Objectives of the Subject
 Learning this subject content will develop the ideas with the fundamental
of analytical chemistry among the students.
 It constructs the fundamental methodology to prepare different strength
of
solutions.
 It facilitate the students to predict the sources of mistakes and errors.
 It helps to develop the fundamentals of volumetric analytical skills.
 It peculates the basic knowledge in the principles of electrochemical
analytical techniques.
 The student interpretation skills will be improve by the course content in
terms of choice of analytical techniques to perform the estimation of
different category drugs. 3
Text /Reference books

1. A.H. Beckett and J.B. Stenlake's, Practical Pharmaceutical

Chemistry Vol I and II, Stahlone Press of University of London.
2. A.I. Vogel, Text Book of Quantitative Inorganic analysis.
3. P. Gundu Rao, Inorganic Pharmaceutical Chemistry.
4. Bentley and Driver's Textbook of Pharmaceutical Chemistry.
5. John H. Kennedy, Analytical chemistry principles.
6. Indian Pharmacopoeia

4
Text /Reference books
Books
• Text Books- G. Vidyasagar Text Book of Pharmaceutical Analysis,
• R.M Verma Textbook of Analytical Chemistry,
• Ashutosh Kar book of Pharmaceutical Drug Analysis,
• S. Ravi Shankar Textbook of Pharmaceutical Analysis
• References books -Indian Pharmacopoeia, Willard Merritt
Dean
Settle

5
Teaching- Learning Process

Total Unit : 05
Each Unit Covered : 07-10 Lectures
Total Lectures : 56
Revision Lecture : 05
Old Paper Discussion : 05

6
Lesson Plan
Lecture Particular
1. Introduction to subject
Module 1 Unit 1: Definition & Scope of Pharmaceutical Analysis (10hrs)
2. Pharmaceutical analysis: Definition & scope; Different analytical
techniques
3. Various methods of expressing concentration
4. Continuation of Various methods of expressing concentration
5. Primary and secondary standards
6. Preparation and standardization of various molar and normal solutions:
oxalic acid, sodium hydroxide, hydrochloric acid
7. Continuation with sodium thiosulphate, sulphuric acid, potassium
permanganate and ceric ammonium sulphate
8. Errors: Sources of errors, types of errors, methods of minimizing errors
9. Accuracy, precision and significant
10. Pharmacopoeia, Sources of impurities in medicinal agents, limit tests
11. Various types of limit tests like Iron, Chloride and sulphate
12 Revision
7
Lesson Plan
Summary
Definition & scope
Methods of expressing Primary and
concentration secondary standards

Module 1
Unit 1

Pharmacopoeia, Errors, Accuracy

agents, limit tests and precision

8
Lesson Plan
Module 2 Unit- II: Acid base titration & Non-aqueous titration (10hrs)
13. Introduction about titrations, end point and equivalent point
14. Theories of acid base indicators
15. Classification of various types of acid base titrations
16. Theory involved in titrations of: Strong Acid Vs Strong Base,
Weak Acid Vs Strong Base
Strong Acid Vs Weak Base & Weak acid-weak base. neutralization
17.
curves
18. Non aqueous titration introduction and principle
19. Various types of non-aqueous solvents
20. Acidimetry and alkalimetry titration
21. Estimation of Sodium benzoate
22. Estimation of Ephedrine hydrochloride
23. Revision

9
Lesson Plan
Summary
Acid base
titration, end Theories of acid
point base
indicators
Module 2
Unit 2

Estimation using
non-aqueous Non-aqueous
titration titration

10
Lesson Plan
Module 3 Unit- III Precipitation, Complexometric, Gravimetry and Diazotization
Titrations (10hrs)
24. Precipitation titrations: Introduction, Mohr’s method, Volhard’s method
25. Modified Volhard’s method Fajan’s method and estimation of sodium
chloride.
26. Complexometric titration: Introduction, type of complexing agents and
classification
27. Applications, masking and demasking reagents
28. Estimation of Magnesium sulphate and calcium gluconate
29. Gravimetry analysis: Introduction, principle involved and types of
gravimetric analysis.
30. Different steps involved in gravimetric analysis, Purity of the precipitate:
co-precipitation and post precipitation,
31. Estimation of barium sulphate
32. Diazotization titration: Introduction and basic Principle
33. Different methods and application of diazotization titration
34. Revision
11
Lesson Plan
Summary

Precipitatio Complexometric
n titration
titration
Module 3
Unit 3

Diazotization Gravimetry
titration titration

12
Lesson Plan
Module 4 Unit IV Redox titrations (08hrs)
35. Introduction of redox titrations
36. Concepts of oxidation and reduction
37. Principle, types of redox titrations and its applications.
38. Cerimetry titration
39. Iodimetry and Iodometry titration
40. Bromatometry titration.
41. Dichrometry titration
42. Titration using potassium iodate.
43. Revision

13
Lesson Plan
Summary

Cerimetry
Redox titration
titration

Module 4
Unit 4

Bromatometry & Iodimetry and

Dichrometry Iodometry
titration titration

14
Lesson Plan
Module 5 Unit- V Electrochemical methods of analysis (07hrs)

44. Conductometry titration: Introduction, conductivity cell

45. Conductometric titrations principle and its applications
46. Potentiometry titrations: Introduction, principle and electrochemical cell
47. Construction and working of reference (Standard hydrogen, silver chloride electrode
and calomel electrode)
48. Indicator electrodes (metal electrodes and glass electrode), methods to determine end
point of potentiometric titration and applications.
49. Polarography: Introduction, principle, application and Ilkovic equation
50. Construction and working of dropping mercury electrode and rotating platinum
electrode
51. Revision
52. Old question Paper
53. Old question Paper
54. Old question Paper
55. Old question Paper
56. Old question Paper

15
Lesson Plan
Summary

Conductometry Potentiometry
titration titrations

Module 4
Electrochemical
methods

Amperometry Polarography

16
 Pharmaceutical Analysis-I
Definition, scope and different
analytical
techniques

Prepared By
Ram Kumar
Assistant Professor
DOPST
MRSPTU, Bathinda
Objectives of the topic
Upon completion of the topic one is be able to Know

 Understands the various scope and concepts of the pharmaceutical analysis in

pharmaceutical drug industry.

18
Lecture
Design
1. Introduction
a. Definition
b. Scope of Pharmaceutical analysis
2. Type and Classification of various technique of pharmaceutical
analysis
3. Importance/ Application of pharmaceutical analysis
4. References
5. Questions

19
Pharmaceutical
Analysis
1. Introduction

a. 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.

20
Pharmaceutical
Analysis
1. Introduction

b. Scope of Pharmaceutical analysis

 Pharmaceutical analysis is integral part of pharma industry not only

research but even pharma manufacturing is incomplete and of no use

without analysis.

 Analyst have huge scope in analytical method development and routine

stability analysis at research centres of all pharma organizations.

21
Pharmaceutical
Analysis
1. Introduction

b. Scope of Pharmaceutical analysis

 At plant analyst are required in documentation and analysis in quality

control and stability departments.

 Apart from this they have significant role in Regulatory department of

pharma companies to check the analytical part of the documents which

needs to be submitted to regulatory authorities.

22
Pharmaceutical
Analysis
Types on basis of analyte size:

Macro Analysis-(0.1 g or more)

Meso (Semi micro) Analysis-(0.01 to 0.1g)

Micro Analysis-(0.001g to 0.01g)

Sub micro Analysis-(0.0001g to 0.001g)

Ultra micro Analysis-(0.0001g)

Trace analysis-(100 to 10000 ppm)

23
Pharmaceutical Analysis
There are main two types of chemical analysis:

 Qualitative (identification)
 It is performed to establish composition of natural/synthetic substances.
These tests are carried out 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.

24
Pharmaceutical Analysis
There are main two types of chemical analysis:

 Quantitative (estimation)
 These techniques are used to quantify any compound or
mainly
substance in the sample.
 These techniques are based upon:
 The quantitative performance of suitable chemical reaction and
either measuring the amount of reagent added to complete the reaction.
 Electrical measurement
 Some spectroscopic properties of the compound

25
Pharmaceutical Analysis

26
Pharmaceutical Analysis
Classification of various analytical methods

 Chemical methods

 Electrical methods

 Instrumental methods

 Biological and microbiological

27
Pharmaceutical Analysis
Chemical methods

Chemical
methods

Volumetri
c or Gravimetric Gasometric
titrimetric methods analysis
methods

Acid Non- Precipitati

Complexometric Diazotisation Redox
base aqueous on
titration titration titrations
titration titrations
titration
28
Pharmaceutical Analysis
 Titrimetric or volumetric method: It is a method used to determine the
concentration of particular solution, by measuring how much of a solution
of known concentration reacts with a known volume od it. Volumetric
methods require simple and less apparatus and they are susceptible of high
accuracy.

 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.

29
Apparatus used for
•titration
Volumetric Flasks
• Burettes
• Pipettes
• Droppers
• Measuring Cylinders
• Wash bottles
• Funnel

Volumetric flask
Burette
30
 Dropper Pipette Funnel

Measuring cylinder Wash bottles

31
Pharmaceutical Analysis

 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.

32
Pharmaceutical Analysis
Electrical methods

Potentiometry

Electrical methods
Conductometry

Polarography

Voltametry

Amperometry

33
Pharmaceutical Analysis

 Electrical methods of analysis involve the measurement of electric current,

voltage or resistance in relation to the concentration of some species in the
solution.
 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.

34
Pharmaceutical Analysis
Instrumental methods

 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.

35
Pharmaceutical Analysis
Example of Instrumental methods

 Spectroscopic methods of analysis depend upon measurement of the

amount of radiant energy of a particular wavelength emitted by the
sample.

 UV-visible Spectroscopy
 Infra red Spectroscopy
 Atomic absorption Spectroscopy
 Nuclear magnetic resonance spectroscopy

36
Pharmaceutical Analysis
Example of Instrumental methods

 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 spectroscopy
 Flame photometry Spectroscopy
 Fluorimetry Spectroscopy

37
Pharmaceutical Analysis
Example of Instrumental methods

 Chromatographic techniques and electrophoretic methods are separation

methods for the mixture of compounds, but also applied for identification
of compounds of mixtures.

 Gas Chromatography (GC)

 High Performance Liquid Chromatography (HPLC)
 Thin Layer Chromatography (TLC)
 High-performance thin-layer chromatography (HPTLC)

38
Pharmaceutical Analysis

UV
spectrophotometer IR spectrophotometer

39
Pharmaceutical Analysis

HPLC NMR

40
Pharmaceutical Analysis
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
called bio-assays.
 Microbiological methods are used to observe potency of antibiotic or anti-
microbial agents.

41
Pharmaceutical Analysis

Importance/Application of Pharmaceutical
Analysis

 Identification of raw materials (in-process and finished product).

 Determination of additional impurities.
 Stability of the drug.
 Strength and concentration of the chemical compound.
 Determine molecular weight of the chemical compound.
 Structure elucidation of synthetic compound.

42
References
 A.H. Beckett and J.B. Stenlake's, Practical Pharmaceutical Chemistry Vol I

and II, Stahlone Press of University of London.

 G. Vidyasagar “Text Book of Pharmaceutical Analysis”, Kalyani publishers,

Vol 1, Ist edition, 2005, Page no. – 1-12

 R.M Verma Textbook of Analytical Chemistry, CBS Publishers, 3rd edition,

2008, Page no. 3-12

 Ashutosh Kar “Pharmaceutical Analysis” CBS Publishers, Volume 1, Ist

edition, 2010, Page no. 3- 7

43
Questions
Short questions
1. Define pharmaceutical analysis. Give its scope.
2. Name different techniques of analysis.
3. What do you understand by volumetric analysis?
4. Define qualitative analysis.
5. Define quantitative analysis.

Long questions
6. Explain different techniques of analysis with suitable examples.
7. Give a comparative characteristic features of various
analytical techniques.
8. Quantitative analysis- In the quality of drugs. Justify the statement with
logical explanations.
44
THANKS