Daniel Yzazel Abayon

QUALITATIVE-QUANTITATIVE
CHEMISTRY
Also known as Analytical
Chemistry or Pharmaceutical
Chemistry
If sample is a drug: Assay
Branch of chemistry which
provides information relative to the
composition of matter
Divisions of Analytical Chemistry
QUALITATIVE
Involves the identification
Composition determination
Ascertainment of impurities
present in a given sample
Answers the question: What is
present in a given sample?
2. QUANTITATIVE
The number or amount
Determination of the proportion of
components in a given sample
Answers the question: How much
is present in the sample?
1.
-

Quantitative Pharmaceutical
Chemistry
The application of procedures
of quantitative analytical
chemistry to the:
Analysis and determination of
purity and quality of drugs and
chemicals used in pharmacy,
Analysis of chemical
constituents found in the human
body,
Analysis of medicinal agents and
metabolites found in biological
systems
Quantitative Analysis
Deals with the methods of
determining the amounts of various
substances or constituents in a
given sample
Volumetric

Ph3B

Quality Control 1
Gravimetric
Special Methods
Physico-chemical

Volumetric Method
- The determination of the volume
of a solution of known
concentration required to react
with a given amount of
substance to be analyzed
Gravimetric Method
- The separation by extraction,
precipitation or other means of
the constituent to be determined
either in the natural state or in
the state of a definite compound
of known composition and the
weighing of the resulting product
Special Method
- Those which require a distinct
type of technique

Analysis of crude drugs

Assay of fats and fixed oils
Assay of volatile oils
Assay of alkaloids
Physico-chemical Method
- Based on some specific physical
and chemical properties of the
substance being analyzed
- Also called Instrumental
method

Daniel Yzazel Abayon

Classification of Analysis
1. Based on Sample size
2. Based on extent of determination
3. Based on nature of methods
4. Based on materials used
Based on sample size
Ultra micro <1 mg
Micro 1 mg 10 mg
Semi-micro 10 mg 100 mg
Macro >100 mg
Based on extent of determination
Proximate total amount of class or
group of active plant principles in a
given sample
Ultimate amount of specific
compartment or single chemical
species present in a sample
Based on nature of methods
Classical (aka general or chemical)
e.g. Titrimetric analysis, Gravimetric
analysis
Instrumentation based on specific
physical or chemical properties of the
analyte; more accurate analysis
e.g. Spectrophotometry, Polarimetry,
Chromatography
Miscellaneous or Specific Method
involves crude drugs and natural
products derived from them
e.g.Water content, Ash content, Acid
value
QUALITY
-

The combination of attributes or

characteristics of a product which,
when compared to a standard, serves
as a basis for measuring the
uniformity of the product and
determines its degree of acceptability
As applied to a drug product, it has
been defined as the sum of all factors

Ph3B

Quality Control 1

that contribute directly or indirectly to

the safety, effectiveness, and
reliability of the product
- Totality of characteristic or features
of a product that bears on its
capacity to satisfy stated or
applied needs
QUALITY CONTROL
- Is a tool which gives the assurance
that a product conforms to
standards and specifications
through a system of inspection,
analysis and action
Quality control guarantees
within limits that a drug
product:
Is free of impurities
Is physically and chemically
stable
Contains the amount of
active ingredients as stated
on the label
Provides optimal release of
active ingredients when the
product is administered
3 main areas of Quality control
1. RMQC Raw Materials Quality
Control
2. IPQC In-Process Quality Control
3. FPQC Finish Product Quality
Control
GENERAL METHODS,
EQUIPMENT AND CHEMICALS
USED IN OFFICIAL
PHARMACEUTICAL
ANALYSIS/ASSAY
CONSTANTS WEIGHT- the official
methods are often direct that a
drug to be dried to constant

Daniel Yzazel Abayon

weight. The term dried to constant
weight means that two
consecutive weighing do not differ
by more than 0.5mg/g of
substance taken for the
determination, the second
weighing following an additional
hour of drying .
An object is said to be at constant
weight when two consecutive
weighing after heating and cooling
do not differ by more than 0.2mg
(if the change in weight in weight
is more than 0.2mg, the process of
heating, cooling and weighing is
repeated until constant weight is
obtained)
Digestion
A process where finely divided
crystalline precipitate is allowed to
stand in contact with the hot
supernatant solution for a
considerable period of time before
filtration. This method permits the
smaller particles to increase in size
(due to greater solubility of smaller
particles over that of larger
particles) thus be retained by the
filter.
Likewise, co-precipitation effects
are lesser and the precipitate
becomes corresponding purer. The
term is also used to denote the
treatment of a substance with a
solution over an extended period
of time.

Ph3B

Quality Control 1

either thru the mouthpiece ot thru

the jet; it is used to wash ppt.
CLEANING SOLUTION
A good cleaning solution for a
glassware can be prepared by
dissolving 200g of sodium
dichromate in 100ml of water
and then adding 1500ml of
sulphuric acid slowly with
stirring.
This solution should be stored in a
thick-walled, glass-stoppered
bottle and used repeatedly foe
cleaning glass and porcelain ware
until it deposits a large amount of
solid material and turns green

POLICEMAN
A piece of soft rubber tubing
(about 3cm long) fitted to the end
of a glass rod with about 2cm
projecting beyond the rod.
It is used to loosen the walls of the
containing vessel adhering
particles that are not removable
by a stream of water from the
wash bottle. It is not be used as
stirring rod or allowed to remain in
analytical solutions.
REAGENTS
Technical; Commercial Grade

CLEANING:
Wash bottle one of the most
useful tools of quantitative
analysis, is used principally to
deliver to a graduate, pipette,
volumetric flask or other container
a small quantity of distilled water,

- Has been subjected to only

superficial purification and is
seldom used in analytical work
except for such purposes as
preparing cleaning solution

Daniel Yzazel Abayon

USP/NF Grade

Ph3B

Quality Control 1

- Conform to the standards set up

by USP/NF. Such chemical are used
more often by the pharmacist by
than the chemist, since more
attention is paid in impurities,
which would make substance unfit
for medicinal use than to
impurities affecting its chemical
use. It is usually inadvisable to use
such chemicals for precise and
analytical purposes.

- Also known as "REAGENT GRADE

CHEMICALS", "CERTIFIED
REAGENT", "TESTED PURITY
REAGENT". The analysis of a
reagent of this type is given either
in terms of the actual percentages
of impurities present or in terms of
the maximum limiting percentages
of the various impurities. This
chemical has a statement on its
label that is conforms to American
Chemical Society (A.C.S)
specifications.

Chemically Pure (CP) Reagent

Primary Standard Grade

- A high degrees of purity, probably

to the extent that the amounts of
impurities are too small to cause
interference in the process in
which the reagent is used.

- A chemical of such purity that it

can be weighed out and used to
standardize a solution to a very
high degree of accuracy. It has a
purity greater than 99.95%

Analytical Reagent Grade (AR)

VOLUMETRIC/TITRIMETRIC

- Reagents which have been

analyzed by the manufacturer and
the analyses of which are given on
the label of the containers and are
favored by the analytical chemist.

- Process wherein the volume of

the solution of known
concentration is taken as a
measure of determining the
amount of active constituent in the
sample.

TITRAND/TITRATE/ANALYTE/ACT
IVE CONSTITUENT
- Chemical substance being
analyzed
Analytical Reagent Grade (AR)
TITRANT

Daniel Yzazel Abayon

Ph3B

Quality Control 1

- Solution of known concentration

SECONDARY STANDARD

TITRATION

- A standard solution used in

indirect or secondary
standardization purposes.

- Process of adding and and

measuring the volume of titrant
used in the assay. It is a process
whereby a standard is brought into
reaction.

EQUIVALENCE POINT/
STOICHIOMETRIC POINT
- The theoretical point at which
equal amounts of analyte and
titrant reacted.

STANDARDIZATION
- Determination the exact
concentration of a solution

VISUAL END POINT/

EXPERIMENTAL END POINT
- Point at which the titration is
stopped and is indicated by a
sudden change in some property
of the reaction mixture; this is
determined by the use of an
indicator or a potentiometer.

STANDARD SOLUTION
- Is a solution, the concentration of
which is known to a high degree of
accuracy. It is also known as
VOLUMETRIC SOLUTION is
commonly referred to by the
abbreviation "VS".

(INSERT TABLE HERE)

PRIMARY STANDARD

INDICATOR- Complex, organic

substance that show when the end
point of a reaction has been
reached, either by: (a) a change in
color (appearance and
disappearance) (b) evolution of a
gas or (c) formation of a
precipitate.

- Substance of high degree of

purity and used in direct
standardization purposes.

TITER- the weight of a substance

chemically equivalent to 1ml of a
standard solution.
BURET OR BURETTE graduated
glass tubes of uniform bore

Daniel Yzazel Abayon

throughout the whole length, used
in the measurement of variables
quantities of liquid. Graduated into
milliliters and tenth milliliters are
closed at the bottom by a glass or
Teflon stop lock to control the
outflow of liquid.
Consist of calibrated tube to hold
the titrant plus a valve
arrangement by which the flow of
titrant is controlled. This valve is
the principal source of difference
among burets.
TYPES OF BURET:
PLAIN OR MOHRS BURET with
pinchcock valve that consist of a
close-fitting glass bead inside a
short length of rubber tubing that
connects the buret and its tip.
PARALLAX- Is a displacement or
difference in the apparent position
of an object viewed along two
different line of sight and is
measured by the angle or semiangle of inclination between those
two lines. The term is derived from
the greek parallaxis, meaning
alteration
EFFECTS OF PARAMETER READING
BURETS
-Only when the eye is on a level
with the meniscus will the reading
give no parallactic error.
PIPET/PIPETTE- permits transfer
of accurately known volumes from
one container to another. It is use
primarily for taking a definite
fractional part of a given solution.
TYPES OF PIPETS:

Ph3B

Quality Control 1
A. VOLUMETRIC OR
TRANSFER PIPET- deliver
single, fixed volume between
0.5 and 200ml( it is often
marked T.D. to indicate that
is designed to deliver the
specific volume)
B. MEASURING PIPETS
calibrated in convenient
units to permit delivery of
any (variable) volume up to
maximum capacity ranging
from 0.1 to 25ml. Mohr and
serological pipets are
examples of measuring
pipets.
C. EPPENDORF
MICROPIPETTE
D. OSTWARLD-FOLIN PIPET
E. LAMBDA PIPET

VOLUMETRIC FLASK
manufacture with capacities
ranging from 5ml to 5ml and are
usually calibrated to contain a
specific volume when filled to a
line etched on the neck. They are
used for the preparation of
standard solution and for the
dilution of samples to a foxed
volume prior to taking aliquots
with a pipet.
NOTE: volumetric flask are
graduate to contain and not to
deliver, the calibrated volume.
GRADUATED CYLINDER used in
making approximate measures of
volume. They are graduated to
contain a given volume of liquid at
standard temperature.