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12 Special Methods
12 Special Methods
12 Special Methods
Pharmaceutical Analyses
crude drugs and products derived from them
PURPOSES:
1. to establish purity
2. to determine the amount of therapeutically
active constituent present
CLASSIFICATION:
1. Chemical Methods
2. Biological Methods – measure the effects
of drugs upon microbes, animals or
animal tissues
Ash Determination
Ash Content
the residue remaining after incineration
represents the inorganic salts naturally occurring in the drug
and adhering to it
may also include inorganic matter added for the purposes of
adulteration
Ash Determination
furnishes a basis for judging the identity and cleanliness of a
drug
gives information relative to its adulteration with inorganic
matter
GRAVIMETRIC METHOD OF ANALYSIS
careful control of temperature is the most important analytical
factor to regulate
Ash Determination
Total Ash
residue remaining after incineration
% Total Ash = ( wt TA / wt sx ) x 100
Acid-Insoluble Ash
part of the total ash which is insoluble in diluted
HCl
consists almost entirely of silica derived from the
soil adhering to the drug
% Acid-Insoluble Ash = ( wt AIA / wt sx ) x 100
Substances with Ash Limits
Residue on Ignition
expensive chemicals
determined by ignition to dull redness
yields negligible amount of ash
quantity not exceeding 500 µg
residue on ignition limits
acetazolamide - upper residue limit of 0.1%
aspirin – upper residue limit of 0.05%
cocaine HCl – residue which remains must not exceed
500 µg
Ash Determination
Loss on Ignition
technique which provides a means of determining the
percentage of test material which is volatilized and driven
off under the conditions specified
definite limitations on the amounts of volatile matter they
will lose when heated
permitted loss in percent weight
USP calamine (2.0), magnesium sulfate (40.0 to 52.0)
NF calcium phosphate tribasic (8.0), kaolin (15.0)
Water Determination
Computation:
1. Gravimetric Method A
for drugs containing no constituents, other than
water, volatile at 105oC
2. Gravimetric Method B
for drugs containing ether-soluble constituents
volatile at 105oC
continuous extraction
uses the same portion
of solvent repeatedly
separation of the
solvent and solute after
the extraction
Solvents for Extraction
Solvents Drugs containing Extractive
1. Absolute Ether Volatile Oils Total Ether –Soluble
Volatile Extrractives
(TESVE)
1.
Extract about 10-g of Cocoa, accurately weighed, with absolute ether in a
continuous extraction apparatus for 8 hours.
2.
Allow the ether solution to evaporate spontaneously in a suitable tared
container, dry at 105oC for 1 hour, and weigh the NVESE.
3.
The ether-insoluble residue is dried at 105oC for 1 hours and tests for total ash,
crude fiber, etc. may be made.
Notes:
8 hours extraction – ensure complete removal of the ether-soluble constituents
from the powdered cocoa
ordinary ether contains water which dissolves some tannin, sugar, etc.
ether boils 35oC
Residue = Ether-Soluble Extractive (ESE) consists of fixed oil and resin
residue heated at 105oC , volatile substances are volatilized
Non-Volatile Ether Soluble Extractive (NVESE) consists of resin, coloring
matter and fixed oil
Ether-Insoluble Residue (EIR)
drying to constant weight:
drying and weighing at 1-hour intervals until the loss is not more than
0.25% in 1 hour of drying
Crude Fiber Content
% Crude Fiber
= [ ( wt residue – wt ash ) / wt drug ] x 100
Constants of
Fats, Fatty Oils, Waxes, Balsams, Resins, etc.
SV = AV + EV
UNSAPONIFIABLE MATTER
Classification of Oils
a. DRYING OIL
very high iodine value
usually above 120
b. SEMI-DRYING OIL
intermediate iodine value
between 100 and 120
c. NON-DRYING OIL
relatively low iodine value
below 100
N.B.
In case of animal fats, iodine value is not very high, usually
being less than 90.
IODINE VALUE [ Iodine Number ]
Computation:
% by volume = mL CF 1 + mL CF 2
ASSAY OF VOLATILE OILS
[ ETHEREAL OILS ; ESSENTIAL OILS ; ESSENCES ]
1. Bisulfite Method
form addition products with certain reagents
bisulfite addition product dissolve in water
non-aldehyde constituents as a water insoluble layer
(residual layer)
CASSIA FLASK
2. Hydroxylamine Method
very small amounts of aldehydes
contain other constituents that form water-soluble
addition products
INDIRECT ALKALIMETRIC METHOD (w/ Blank
Test)
ASSAY FOR KETONE CONTENT
2. Hydroxylamine Method
INDIRECT ALKALIMETRIC METHOD (w/ Blank
Test)
ASSAY FOR PHENOL CONTENT
CASSIA FLASK
DETERMINATION OF VOLATILE OIL CONTENT
OF CRUDE DRUGS AND OLEORESINS
BABCOCK BOTTLE
1 division = 0.2-mL
properties of alkaloids
free alkaloids – sparingly soluble in water ; readily
soluble in immiscible solvents
alkaloidal salts – readily soluble in water ; sparingly
soluble in immiscible solvents
combine with acids to form salts
liberated from aqueous solutions of their salts by alkali
form highly insoluble precipitates with a number of reagents
ASSAY OF ALKALOIDS AND AMINE DRUGS