Introduction to Pharmaceutical analysis - I (HRB)

Pharmaceutical
analysis
PRESENTED BY:-
Miss.- Harshada R. Bafna.
M. Pharmacy.(Q.A.)

Contents-
• Definition and scope Pharmaceutical analysis.
• Different techniques of analysis.
• Methods of expressing concentration.
• Primary and secondary standards.
• Errors: Sources of errors, types of errors, methods of
minimizing errors, accuracy, precision and significant figures.
• Pharmacopoeia.
• Sources of impurities in medicinal agent.
• limit tests.
29/14/2020 Pharmaceutical analysis.(HRB)

Pharmaceutical analysis
3
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
Scopes of analysis
1. In pharmaceutical industry- There are different sectors in
pharmaceutical industry as research and development (R&D) and
Quality control (QC) in which pharmaceutical analysis is utilizes
regularly.
2. In Food industry- As we all know packed food which consumed
by consumer should have all parameters like quality, purity and
safety which enhance acceptability by consumer. For this it is
require analyzing all these parameters for packed food.

4
Different kind of preservatives,coloring, flavorings and sweetening
agents are used in packed food which can be a natural or synthetic
chemical ingredient so these should analyze qualitatively and
quantitatively, for this various kind of analytical techniques can be
applicable.
3. In Cosmetic Industry- Preparation of cosmetics, as lipsticks,
creams, nail paints, lotions, shampoo and conditioners etc., play with
two things as colour and odour and these colouring agents and
fragrances are also build by different chemical ingredients so the
quality and quantity of these ingredients should be known which can
be analyse by different techniques of analysis
4.In Disease diagnosis- Different diseases can be diagnosed by
pharmaceutical analysis techniques like HIV is observed by ELISA
method

Different techniques of analysis
9/14/2020 Pharmaceutical analysis.(HRB) 5
There are main two types of chemical analysis.
1. Qualitative analysis (identification)
2. Quantitative analysis (estimation)
Qualitative analysis 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.
Quantitative analytical : Techniques are mainly used to quantify
any compound or substance in the sample.

ANALYTICAL TECHNIQUES CLASSIFIED IN
TO THE FOLLOWING CATEGORIES
Volumetric
Analysis
Electrochemical
Analysis
Spectroscopic
Analysis
Chromatographic
Analysis

Volumetric method of analysis:
as name is clear that in this titration volume is used. So
it is quantitative methods.
Volumetric analysis classified in to
1. Acid – base titration
a)Aqueous titration
b) Non aqueous titration
2. Redox titration
3. Complexometric titration
4. Precipitation titration
Volumetric Analysis

Electrochemical Analysis
Electrochemical methods: are analytical techniques that
use a measurement of potential, charge, or current to
determine an analyte’s concentration.
1.Potentiometric
2.Conductometric
3.Amperometric
4.Polarography

Spectroscopic Analysis
Spectral analysis: Spectroscopy can involve any interaction
between light and matter, including absorption, emission,
scattering, etc.
 Four techniques commonly used to help with structural
analysis:
1.Ultraviolet-visible spectroscopy(UV)
2.Infrared spectroscopy (IR)
3.Nuclear Magnetic Resonance Spectroscopy (NMR)
4.Mass spectrometry

Chromatographic Analysis
Chromatographic analysis: Chromatography' is an analytical
technique commonly used for separating a mixture of chemical
substances into its individual components.

Primary and secondary standards
Primary Standards

Secondary standard
 Secondary standard is a chemical that has
been standardized against a primary
standard for use in a specific analysis.
 Secondary standards are commonly used to
calibrate analytical methods.
 A secondary standard is a substance which
may be usedfor standardization.
 A secondary standard is a standard that is
prepared in the laboratory for a specific
analysis.

Methods of expressing concentration.
In all the techniques of quantitative
analysis the use of solutions requires some
basis for the expression of solution
concentration.
1. Normality
2. Molarity
3. Molality
4. Percent Solution
5. Formal Concentration
6. Parts per Million (PPM)

Normality- Number of gram equivalent of solute (Substance)
dissolved in one liter (1000 ml) of solution is called as Normality.
Normality is indicated by N
Gram equivalent Weight of Solute
Equivalent Weight = ---------------------------------------------
No. of replaceable H + & OH -
Normality Examples-
1) NaOH -
1.Molecular weight of NaOH (Sodium Hydroxide)=
Atomic Weight of Na = 22.99
Atomic Weight of O = 16
Atomic Weight of H = 1
Total = 40
Normality

2. Normality-
1N = 40 gm of NaOH is Dissolved in 1000 ml of water
(H2O)
0.1 N = 4 gm of NaOH is Dissolved in 1000 ml of water
(H2O)
0.01N = 0.4 gm of NaOH is Dissolved in 1000 ml of water
(H2O)

Molarity
Molarity - Number of moles of solute (Substance) dissolved in
one liter (1000 mL) of Solution is called as Molarity.
 1 gm in 1000 ml = 1 mol.
 Molarity is indicated by M
Number of moles of Solute
M =
1000 mL of Solution
Molarity Examples-
1) NaOH -
1. Molecular weight of NaOH (Sodium Hydroxide)=
Atomic Weight of Na= 22.99
Atomic Weight of O= 16
Atomic Weight of H= 1
40

2. Molarity -
1M= 40 gm of NaOH is Dissolved in 1000 mL of water (H2O)
0.1 M= 4 gm of NaOH is Dissolved in 1000 mL of water (H2O)
0.01M= 0.4 gm of NaOH is Dissolved in 1000 mL of water (H2O)
2) HCl
1.Molecular weight of HCl (Hydrochloric acid) =
Atomic Weight of Cl = 35.5
Atomic Weight of H = 1
Total 36.5
2.Molarity -
1M = 36.5 gm of HCl is Dissolved in 1000 mL of water (H2O)
0.1 M = 3.65 gm of HCl is Dissolved in 1000 mL of water (H2O)
0.01M = 0.365 gm of HCl is Dissolved in 1000 mL of water (H2O)

20
Molality- A molar solution contains 1 mole of solute per one
kilogram of solution ( 1 lit. of solvent) is called as Molality.
 Molality is indicated by M
Number of mol. Wt. of substance
M =
1000 gm of Solution (1Kg)
Molality Examples-
1) NaOH -
1. Molecular weight of NaOH (Sodium Hydroxide)=
Atomic Weight of Na= 22.99
Atomic Weight of O= 16
Atomic Weight of H= 1
40
Molality

2. Molality-
1 M = 40 gm of NaOH is Dissolved in 1000 gm of water
(H2O)
0.1 M = 4 gm of NaOH is Dissolved in 1000 gm of water
(H2O)
0.01 M= 0.4 gm of NaOH is Dissolved in 1000 gm of water
(H2O)
1.5 M= 60 gm of NaOH is Dissolved in 1000 gm of water
(H2O)

Percent (%) Solution
Percent (%) Solution
 Sometimes the concentration is expressed in terms of per cent
(parts per hundred) also.
 Per cent Composition of a solution can be expressed as:
1. Per cent W/W = Weight of solute/ Weight of solution X 100
2. Per cent V/V = Volume of solute/ Volume of solution X 100
3. Per cent W/V= Weight of solute/ Volume of solution X 100
 1 %= 1gm of KCl ----------- in 100 ml of water
10 % = 10 gm of KCl ----------- in 100 ml of water
100 % = 100 gm of KCl ----------- in 100 ml of water

Formal Concentration
 The concentration unit, formal, is similar to the more familiar
molar concentration in that it is calculated as the number of
moles of a substance in a liter of solution.
 Formal concentrations are notated with the symbol F.
 The formal Concentration (Formality) is applicable to the ionic
Substances.
Ex. 1. Calcium carbonate (100 g/mole).
If one has 1 g CaCO3 in 1 L aqueous solution, the concentration
of CaCO3, in formal, is...
1 g CaCO3/(100 g CaCO3/mole)/(1 L) = 0.01 F CaCO3

Parts Per Million
Parts per million is frequently employed to express the
concentration of very dilute solutions and is express as PPM .
Mass of solute
Conc. In PPM = × 106 PPM
Mass of solution
 1 PPPM = 1 mg/it.

Errors
Error is the difference between the true result and the
measured result.

The gross error occurs because of the human mistakes.
For examples consider the person using the instruments takes the
wrong reading, or they can record the incorrect data.
Such type of error comes under the gross error. The gross error
can only be avoided by taking the reading carefully.
Two methods can remove the gross error.
These methods are
1.The reading should be taken very carefully.
2.Two or more readings should be taken of the measurement
quantity. The readings are taken by the different experimenter and
at a different point for removing the error.
Gross Errors

Systematic Errors
 The systematic errors are mainly classified into three categories.
1.Instrumental Errors
2.Environmental Errors
3.Observational Errors
Instrumental Errors
 These errors mainly arise due to the three main reasons.
(a)Inherent Shortcomings of Instruments – Such types of errors
are inbuilt in instruments because of their mechanical structure.
They may be due to manufacturing, calibration or operation of
the device.

(b) Misuse of Instrument – The error occurs in the instrument
because of the fault of the operator. A good instrument used in an
unintelligent way may give an enormous result.
(c) Loading Effect – It is the most common type of error which is
caused by the instrument in measurement work
Environmental Errors
 These errors are due to the external condition of the measuring
devices. Such types of errors mainly occur due to the effect of
temperature, pressure, humidity, dust, vibration or because of the
magnetic or electrostatic field.

Observational Errors
 Such types of errors are due to the wrong observation of the
reading.
Random Errors
 The error which is caused by the sudden change in the
atmospheric condition, such type of error is called random error.

Methods of minimizing errors
 Gross errors cannot be completely eliminated, but can be
minimized by taking proper care in reading and recording of the
measurement parameter. One should, therefore, not be
completely dependent on a single reading
 Instrumental Systematic errors can be avoided by -
a. selecting a suitable instrument for the particular measurement
applications
b. applying correction factors after determining the amount of
instrumental error
c. calibrating the instrument against a standard

 Environmental Systematic errors can be avoided by air
conditioning, hermetically sealing certain components in the
instruments, and using magnetic shields
 Observational Systematic errors can be avoided by concentrating
on one particular measurement process at a time. Clearing out
the area where the instrument is placed will also help the
observer focus
 Random errors can be treated mathematically using laws of
probability. The idea is to repeat the measurement to gain high
precision.

ACCURACY
 Definition : Closeness of the test results obtained by the method
to the true value.
 Accuracy is inversely proportional to the error.
 The greater the accuracy, smaller is the error.

Precision
 Definition : The closeness of agreement (degree of scatter)
between a series of measurements obtained from multiple
samplings of the same homogeneous sample.
 It should be investigated using homogeneous, authentic samples.
 Precision designates reproducibility of ameasurement, whereas
accuracy the correctness of a measurement.

PHARMACOPOEIA
Pharmacopoeia
 Derived from Greek word ‘Pharmakon’ means drug and
‘Poiea’ means to make.
 It is a legal and official book issued by recognized authorities
usually appointed by Government of each country.
 It comprises list of pharmaceutical substances, formulae along
with their description and standards.
 List of Pharmacopeias:
a) Argentine b) Austrian c) Belgian d) Brazilian e) British
f) Chinese g) Egyptian h) European i) French j) German
k) Hungarian l) Indian m) International n) Italian o) Japanese
p) Yugoslavian q) Mexican r) Netherlands s) Nordic t) Polish
u) Portuguese v) Rumanian w) Russian

The pharmacopoeia contain-:
1. List of drug and other related substances
2. Sources
3. Description
4. Tests
5. Formulas for preparation actions
6. Uses
7. Doses
8. Storage

Indian Pharmacopoeia
 The process of publishing the first Pharmacopoeia started in the
year 1944 under the chairmanship of Col. R. N. Chopra
 In 1948 government of India appointed an Indian Pharmacopeia
committee for preparing ‘Pharmacopeia of India’.
 1st edition I. P. 1955 was published in the official gazette. Dr. B.
N. Ghosh, Chairman
– Supplement 1960
 2nd edition I. P. 1966, Dr. B. Mukherji, Chairman, Shankar S.
– Supplement 1975
 3rd edition I. P. 1985, Dr. Nityanand, Chairman
– I Addendum/Supplement 1989
– II Addendum/Supplement 1991

 The British Pharmacopoeia (BP) is the national pharmacopoeia
of the United Kingdom.
 The British Pharmacopoeia is an important statutory component
in the control of medicines. Along with the British National
Formulary (BNF), it defines the UK’s pharmaceutical standards.
British Pharmacopoeia
4th edition I. P. 1996 Dr. Nityanand, Chairman
– III Addendum/ Supplement 2000
– IV Addendum/ Supplement 2002
5th edition I. P., 2007, Dr. Nityanand, Chairman
 6th edition I. P., 2010
 7th edition I. P. 2014V Addendum/Supplement 2015

European Pharmacopoeia
The European Pharmacopoeia is a pharmacopoeia that aims to
provide common quality standards throughout Europe to control
the quality of medicines and the substances used to manufacture
them.

Sources of impurities in medicinal agent
 Impurities which have toxic effects on body and bring about
unpleasant reactions when present beyond certain limits. e.g
Lead and Arsenic salts.
 The impurities which are able to make substance incompatible
with other substances.
 The impurities which if present beyond the limit, affect the
storage property of the pharmaceuticals.
 The impurities which are harmless, but if present beyond the
limit, it will lower the active strength of the medicinal
compound. E.g. Sodium salt in potassium salt.

 The impurities which may bring about technical difficulties in
the use of the substance.
 Impurities such as taste, odour, colour or appearance which can
be easily detected by the senses and make the substance
unhygienic and unaesthetic. E.g. Sodium chloride becomes
damp because of the presence of traces of magnesium salts.
Also phenolic impurities present in sodium salicylate alters its
odour.

Limit tests
Definition: Limit tests are quantitative or semiquantitative
test designed to identify and control small quantities of
impurities which are likely to be present in the substances.
Example- limit test of iron, limit test of sulphur etc.
 Importance's of limit test-
 Tests being used to identify the impurity.
 Tests being used to control the impurity.

Referances
9/14/2020 42
1. A Textbook of Pharmaceutical Analysis (volume – I) by DR A V
Kasture, DR H N More, DR K R Mahadik, DR S G Wadodkar,
Nirali Prakashan, Pg.no. 1-7.
2. A Textbook of Pharmaceutical Analysis by David. G. Watson,
Churchill Livingstone, Pg.no. - 51
3. A.H. Beckett & J.B. Stenlake's, Practical Pharmaceutical
Chemistry Vol I & II, Stahlone Press of University of London.
4. www.google.com.

Limit tests
Definition: Limit tests are quantitative or semiquantitative test
designed to identify and control small quantities of impurities
which are likely to be present in the substances.
 e,g. 1.Limit test of iron.
2.Limit test of arsenic.etc.
 Tests being used to identify the impurity.
 Tests being used to control the impurity.

Introduction to Pharmaceutical analysis - I (HRB)

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