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There are many methods available for the determination of emulsion type but the most
commonly used are:
Drop dilution method.
Dye solubility method.
Fluorescent test.
Electrical conductivity test.
Direction of creaming test.
Filter paper test.
These methods determine whether the emulsion is oil in water (o/w) type or water in
oil (w/o) type.
DROP DILUTION METHOD:
This method is based on the principle that emulsion is always miscible with the
external phase. If water is added to water in oil w/o type emulsion, it will not be
mixed. On the other hand, oil mixes well.
Same is the case with o/w type emulsion. If oil is added to oil in water o/w type
emulsion, it will not be mixed. On the other hand, water mixes well.
DYE SOLUBILITY METHOD:
It is based on the solubility of any dye in the external phase. Amaranth, a water
soluble dye gives color to oil in water o/w type emulsion, but not to water in oil w/o
type emulsion. Same is the case with oil soluble dyes.
FLUORESCENT TEST:
Based on the fluorescence of oils under ultraviolet light, the emulsion is examined
under the light in the microscope. If the whole fluid is fluorescent, it is water in oil
w/o but in case of oil in water o/w spotty fluorescence will appear.
ELECTRICAL CONDUCTIVITY TEST:
Based on the electrical conductivity of aqueous solutions, the electric current is
supplied and electrodes are placed in the emulsion. If the current is passed, it is oil
in water o/w and if is not passed, it is water in oil w/o.
DIRECTION OF CREAMING TEST:
Creaming is the sedimentation of the dispersed phase which is either upwards or
downwards, upon which this test is based. The density of oil is mostly less than
water. Thus if creaming is at the upper side, it is oil in water o/w and if it is
downwards, it is water in oil w/o type of emulsion.
FILTER PAPER TEST:
Take a filter paper, put a drop of emulsion on the filter paper. Evaporate it; if there
is a spot on the filter paper, the emulsion will be water in oil w/o. On the other
hand, if there is no spot, the emulsion will be of oil in water o/w type.
DETERMINATION OF TOTAL SOLIDS
The term “total solids” is applied to the residue obtained when the prescribed amount
of the preparations is dried to constant weight under the conditions specified. Total
solids usually include extractives, both soluble and insoluble in alcoholic or hydro-
alcoholic preparations as tinctures and extracts.
The total solids are calculated as g/100ml
This test is more preferably performed for the tinctures or galenical preparations
containing a higher amount of solid contents.
PROCEDURE:
Take a china dish, weigh it then add 5ml of the tincture or the given preparations.
Heat this to evaporation. Then weigh it again.
Increase in weight is the weight of total solids in 5ml of sample.
Specific ranges are given in pharmacopoeia.
EVALUATION OF ELIXIRS
Elixirs are clear sweetened usually hydro-alcoholic liquids containing flavoring
substance.
TESTS FOR THE EVALUATION OF ELIXIR
Following are the tests for the evaluation of elixirs.
Consistency.
pH determination.
Refractive index
Alcoholic contents.
Identification.
Assay of active contents.
CONSISTENCY:
Should be clear.
pH DETERMINATION:
6.0 to 7.0.
REFRACTIVE INDEX:
1.4608-1.4630.
ALCOHOL CONTENTS:
It should be 1 of the percentage given in the monograph.
IDENTIFICATION:
To 5ml add 2ml of 5M NaOH and mix. A liquid with the odour of chloroform is
separated.
ASSAY OF ACTIVE CONTENTS:
To 3 grams add 25 grams of Zinc powder, 15ml of glacial acetic acid.
Add 30ml of water, boil under reflux condenser for 30 minutes, cool, filter through
absorbent cotton, wash the residue with water and combine the filtrate.
Add 20 ml of 2M Nitric acid, wash the residue with water and titrate the excess of
silver nitrate with 0.1M Ammonium Thiocyanate using Ammonium iron sulphate as
an indicator.
Each ml of 0.1M silver Nitrate 0.005513 grams of C2H3Cl3O2.
EVALUATION OF SYRUPS
Syrups are concentrated aqueous solutions having 66.7 % w/v of sucrose. Syrups also
contain aromatic or other flavoring materials.
TESTS FOR EVALUATION OF SYRUPS
Following tests are specified for the evaluation of syrups:
Consistency.
pH determination.
Refractive index.
Identification of active contents.
Assay of active contents.
Solubility.
CONSISTENCY:
Should be clear solution.
There should be no solid particles.
pH DETERMINATION:
Determine the pH of syrup by suitable means; it should be 6.0 to 7.0.
REFRACTIVE INDEX:
The value of refractive index should be in the range of 1.4608 to 1.4630.
IDENTIFICATION OF ACTIVE CONTENTS:
Identify the active contents of syrup by suitable means e.g. invert syrups dissolve
with 10 ml of water and 5ml of potassium cupric tartarate solution. A red precipitate
is produced.
ASSAY OF ACTIVE CONTENTS:
For example, Lemon syrup.
Mix 8 grams with 100ml of water and titrate with 0.1M NaOH using
phenolphthalein as an indicator.
Each ml of 0.1M NaOH=0.007005 grams of C6H8O7.H2O
SOLUBILITY:
Soluble in water.
EVALUATION OF SUPPOSITORIES
Suppositories are semisolid preparations administered through the orifices, each contain
one or more medicaments.
They are normally administered as a single dose for local or systemic action.
TESTS FOR THE EVALUATION OF SUPPOSITORIES
Appropriate test methods and specifications are developed, which are capable of
guaranteeing that the purpose for which suppositories are used will be fulfilled.
TESTS FOR SUPPOSITORIES ARE:
1. Uniformity of weight
2. Disintegration test.
3. Content uniformity test.
4. Melting point determination test.
5. General appearance test.
6. Assay of active contents.
1). UNIFORMITY OF WEIGHT:
Weigh 20 suppositories individually.
Determine their average weight.
Not more than two of individual weights should deviate from the average weight more
than 5% and none deviates by more than 10%.
2). DISINTEGRATION TEST:
APPARATUS: A transparent sleeve of glass or suitable plastic of height 60mm with an
internal diameter of 52mm.
A metal device consisting of two stainless discs each of which contain 39 holes, each
4mm in diameter.
Diameter of the disc is closely similar to the internal diameter of the sleeve.
Discs are separated by a distance of 30mm. Metal device is attached to outer sleeve by
means of three equally spaced hooks.
Method: Place a suppository on the lower perforated disc of metal device and then
insert the device into the cylinder and attach this to the sleeve.
Repeat the same operation with further two suppositories, metal device and sleeve.
Place each piece of apparatus in a vessel containing at least five liters of water at 37C
and fitted with a slow stirrer and by means of holding the top of apparatus 90 mm
below the surface of water. After every 10 minutes invert each apparatus without
removing it from water.
Disintegration is complete when molded suppositories are:
Completely dissolved.
Dispersed into its components.
Have become soft.
Disintegration occurs in not more than 30 minutes for fat based suppositories and for
water-soluble suppositories disintegration occurs in not more than 60 minutes.
3). CONTENT UNIFORMITY TEST:
Take 10 suppositories; determine the active ingredients of each of the 10 suppositories
by using a suitable analytical method.
If not more than one of the individual values thus obtained is outside the limit i.e.
% of the average value and none of them is outside the limit i.e. 25% of the average
value.
Repeat the test by using another 20 suppositories taken at random. If out of 30
suppositories not more than 3 individual values are outside the limit 15% of the
average values and none is outside the limit 25% of the average value, then the test
is O.K, otherwise failed.
4). MELTING POINT DETERMINATION TEST:
Melt the suppositories rapidly at a temperature not more than 10C above the point of
complete fusion. Insert one end of glass capillary tube into the melted substance so
that a column of substance become 8-12 high rise into it. Cool the tube to 15C and
maintain the temperature at 15-17C for not less than 16 hours. Attached the tube to
thermometer in the heating vessel containing water at 15C so that the lower end of the
column of substance is 30mm below the surface of water. Heat the water with constant
stirring, so that the temperature rise at a rate of 2C per minute.
The temperature at which partially melted substance begins to rise in the tube is
regarded as the melting point. The melting point of suppositories should not rise more
than that given in the monograph.
5). GENERAL APPERANCE:
When cut longitudinally, the internal and external surface should be same.
6). ASSAY OF ACTIVE CONTENTS:
Official limit for the active contents is 95- 105% e.g. Glycerol Suppositories.
Dissolve a number of suppositories equivalent to 8 grams of glycerol in 50 ml of water
and add quantity sufficient to produce 250ml.
Take 5ml of this solution and 150ml of water and 0.25ml of Bromocresol purple solution
and add 0.1M.NaOH to neutralize the blue color of indicator.
Add 1.6 grams of sodium metaphenolate and allow to stand for 15 minutes and titrate
with 0.1M NaOH to same blue color.
Each ml of 0.1M NaOH=0.00921 grams of glycerol.
EVALUATION OF OINTMENTS