UNIT I : Part 1.

1
Scope of Pharmaceutical Analysis
Classification of Quantitative Analytical
Techniques
Introduction to Pharmacopoeial
Monograph

Analytical Chemistry
Analytical chemistry is the study of:
Separation ( Mixture)
Identification
Quantification
of the chemical components present in a sample
Analyte = the component(s) of a sample that is to be determined.

BRANCHES OF ANALYTICAL CHEMISTRY

Qualitative
Analysis
(identification)
provides
information about the identity of species or functional
groups in the sample (an analyte can be identified).
e.g recognized by color, boiling point, solubility,
taste

Quantitative Analysis provides numerical information

of analyte (quantitate the exact amount or
concentration).

CLASSIFICATION OF ANALYTICAL METHODS

Refer class notes

classical METHODS
In wet procedures chemical reactions are used to perform the analysis and
there is no use of any mechanical or electronic instrument except of an
analytical balance.

For qualitative analyses, the separated components were

recognized by:
their colors (with or without reaction with a chemical
reagent
boiling points or melting points,
their solubility in a series of solvents
their odors

CLASSICAL METHODS
For quantitative analyses, the amount of analyte is
determined.
Gravimetric Methods Weight of pure analyte or some
compound produced from the analyte is determined.
Weight is measured directly
Volumetric /Titrimetric Methods the volume of a
standard reagent required to react completely with the
analyte is measured . Volume is correlated with weight of
analyte
Eg Acid-base (neutralization) , Complexometric , Redox etc

INSTRUMENTAL METHODS (physicochemical

methods)

Ininstrumental proceduresthere is use of

instruments of some sort. e.g colorimeter

TYPES OF INSTRUMENTAL
ANALYSIS

PROPERTY MEASURED

SPECTROMETRIC : ABSORBTION
e. g UV , VISIBLE (COLORIMETRY),IR, NMR

INTENSITY OF EMR ABSORBED BY ANALYTE

SPECTROMETRIC: FLUORESCENCE
E.g FLUORESCENCE

INTENSITY OF EMR EMITTED BY ANALYTE

SPECTROMETRIC : SCATTERING
E.g RAMAN , NEPHLOMETRY , TURBIDIMETRY

SCATTERED RADIATION MEASURED

ELECTROCHEMICAL
E.g POLARIGRAPHY, AMPEROMETRY,
COULOMETRY , POTENTIOMETRY

ELECTRICAL PROPERTIES OF ANALYTE

MASS SPECTROMETRY

MASS OF MOLECULAR FRAGMENTS

CHROMATOGRAPHIC METHODS
E.g HPLC, GC,HPTLC

SEPRATION AND THEN MEASUREMENT

PHYSICOCHEMICAL PROPERTY OF AN ANALYTE

THERMAL
E.g THERMO GRAVIMETRY,DSC,DTA

PHYSICOCHEMICAL PROPERTY OF ANALYTE IS

MEASURE AS IT IS HEATED OR COOLED

Applications /scope of analysis

1. Bioanalytical: Detection of various elements and substances in body
fluids. (e.g. Cholesterol ,glucose , proteins, amino acids in blood & urine)
Plasma levels of drug administered
2. Environmental: Heavy metals ,pesticides in air, water, soil. These are
present in traces and very sensitive method is required for their
determination
3. Material science: polymers, characterization of new materials
4. Forensic science : analysis related to criminology; DNA finger printing, finger print
detection; blood analysis.
5. Industrial quality control - required by most companies to control product quality :Both
raw materials and finished products are monitored for quality (purity ,
impurity) in food industry and drug industry
e.g assay of bulk drug , assay of drug product

Pharmacopoeial Monograph
Pharmacopoeias are official documents that provide guidelines,
specifications, and analytical procedures for various drug substances & drug
products
Indian Pharmacopoeia (IP)
British Pharmacopoeia (BP)
United states pharmacopoeia (USP)
European Pharmacopoeia
Japanese pharmacopoeia
The minimum standards are prescribed for a chemical in monographs
Drug manufacturers must comply with these pharmacopoeias according to
the regulations of different countries.

Pharmacopoeial Monograph
MONOGRAPH:

DEFINITION:
Monograph : MONO- SINGLE

GRAPH- WRITING

MONOGRPAH is a detailed written study of a single

specialized subject
Each pharmaceutical substance (API , Excipient or FPP)
is described under monograph.

PARTS OF MONOGRAPH
TITLE:
Official Name of the compound
CHEMICAL NAME (in accordance with the IUPAC)

ASPRIN
Synonyms of the compound is given :
ACETYL SALICYLIC ACID
e. g Calcium carbonate - official name
Precipitated Chalk Synonym

CHEMICAL FORMULA & MOLECULAR WEIGHT:

Indicates the chemical composition of the substance

e.g Magnesium Chloride Official Name

Chemical Formula-MgCl2.6H2O
Molecular Weight - 202.3
This information is not given if the composition of substance is uncertain

e.g Ferric ammonium citrate

INFORMATION IN MONOGRAPH
CATEGORY:
Indicates pharmaceutical use of compound
e. g Aspirin - Analgesic
Pharmaceutical aid
DOSAGE:
Dose and route of administration is given
e.g Calcium gluconate - Intramuscular injection 1-2 gms
e.g Aspirin - 300-600 mg four to six times a day
Strength is given
e.g Aspirin Tablets - 75mg, 150mg,300mg,600mg
DOSAGE IS NOT GIVEN FOR SUBSTANCES NOT TO BE GIVEN
INTERNALY

INFORMATION IN MONOGRAPH

DESCRIPTION:
Physical properties
Solid, Semi-solid , Liquid
Colour- Colourless , Brick Red etc
Crystalline or Amorphous
Odour

SOLUBILITY:
Information on solubility

INFORMATION IN MONOGRAPH

IDENTIFICATION :
Involves some specific and other tests for the identity of a
substance. These tests This can be Chemical test OR
INSTRUMENTAL (IR Spectrum)
e.g Aspirin- CHEMICAL TESTS:

PARTS OF MONOGRAPH

IDENTIFICATION :
TEST A: USING IR INSTRUMENT. THIS GENERATES IR SPECTRUM OF
ASPIRIN WHICH IS COMPARED WITH IR SPECTRUM OF STD ASPIRIN
(SPECTRUM OF OFFICIAL DRUGS IS AVAILABLE IN OFFICIAL BOOKS
LIKE PHARMACOPOEIAS

PARTS OF MONOGRAPH
Standards for purity
WHAT IS PURITY????
Mass of PURE compound in an IMPURE
sample
e.g Aspirin Aspirin contains not less
that 99.5% and not more than 100.5%
of aspirin. Thus a given sample is
analysed to find out whether or not the
aspirin contents are with in the stated
range
Provides standards of purity and
strength
Substance must confirm to the
standards given in monograph

PARTS OF MONOGRAPH
TESTS FOR PURITY & LIMITS
FOR IMPURITIES (SPECIAL
TESTS):
Describes the purity standard of a compound
these include chemical tests like limit test for
heavy metals & physical constants
LIMIT TEST: To detect small amounts of impurity
PHYSICAL CONSTANTS:
Help in both identification and maintenance of
standards
Eg melting point, boiling point, specific gravity,
refractive
index(liquids)
,
optical
rotation
(biologically active form), viscosity (oils), swelling
power, polymorphism(solids), acid value ,
saponification value (oils and fats)

INFORMATION IN MONOGRAPH
QUANTITATIVE ASSAYS
The term assay indicates the quantitative determination of principal ingredients of the official
substances and their preparations.
PACKAGING STORAGE AND LABELLING:
Storage conditions of official substance is prescribed.
Light resistant container: substance must be protected against light. amber colored
Well closed: substance must be protected against dust , dirt etc
Tightly closed : substance must be protected against atmospheric oxygen , moisture
Storage conditions:
cold: 2-8 degree
Cool : 8-25 degree
Room temperature
Labelling:
Aspirin tablets dispersible: