1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Amantadine hydrochloride from the
Pharmacopoeial specifications.
2.0 SCOPE:
This
SOP shall be applicable in Q.C laboratory.
3.0 RESPONSIBILITY:
3.1 Q.C Analyst.
4.0 ACCOUNTABILITY:
4.1 Q.C Manager.
5.0 PROCEDURE:
5.1 Characters:
5.1.1
Appearance:
5.1.1.1 White or almost white.
5.1.1.2 Crystalline powder.
5.1.2
Solubility:
5.1.2.1 Material and equipment:
5.1.2.1.1
Glassware
(2 test tubes, 1 spatula).
5.1.2.1.2
Ethanol
(96%).
5.1.2.1.3
Purified
water.
5.1.2.2 Sample:
5.1.2.2.1
Small
quantity.
5.1.2.3 Method:
5.1.2.3.1
Take
2 test tubes and add small quantity of sample for testing solubility according
to B.P specifications.
5.1.2.3.2
Add
purified water in test tube 1 and observe.
5.1.2.3.3
Add
Ethanol (96%) in test tube 2 and observe.
5.1.2.4 Observations:
5.1.2.4.1
The
sample in test tube 1& 2 containing with purified water and ethanol (96%)
are freely soluble.
5.2 Solution
S:
5.2.1
Material
and equipment:
5.2.1.1 Glassware (1 50.0ml of beaker, 1 spatula,
1 glass rod, 1 pipette).
5.2.1.2 Analytical weighing balance.
5.2.1.3 Magnetic stirrer.
5.2.1.4 Carbon-dioxide free water.
5.2.2
Sample:
5.2.2.1 2.5 g.
5.2.3
Preparation
of solution S:
5.2.3.1 Take a beaker of 50.0ml and add sample 2.5g
in it.
5.2.3.2 Add in it sufficient quantity of Carbon-dioxide
free water. And dissolve it by using magnetic stirrer.
5.2.3.3 Dilute it to 25.0ml with the same solvent.
5.3 Identification
tests:
5.3.1
5.3.1.1 Material and equipment:
5.3.1.1.1
Glassware
(according to requirement).
5.3.1.1.2
1.0ml
of 0.1M hydrochloric acid.
5.3.1.1.3
1.0ml
of a 500g/L solution of sodium nitrate.
5.3.1.1.4
Purified
water.
5.3.1.2 Sample:
5.3.1.2.1
0.2g.
5.3.1.3 Method:
5.3.1.3.1
Take
a test tube and add 0.2g of the sample in it.
5.3.1.3.2
Dissolve
the sample by adding 1.0ml of 0.1M hydrochloric acid.
5.3.1.3.3
And
then add 1.0ml of a 500g/L solution of sodium nitrate.
5.3.1.3.4
Observe
the changes.
5.3.1.4 Observations:
5.3.1.4.1
A
white ppt is formed.
5.3.2
Chlorides test:
5.3.2.1 Material and equipment:
5.3.2.1.1
Glassware
(according to requirement).
5.3.2.1.2
Dilute
nitric acid.
5.3.2.1.3
0.4ml
of Silver nitrate R1.
5.3.2.1.4
Ammonia.
5.3.2.1.5
Purified water.
5.3.2.2 Sample:
5.3.2.2.1
1.0ml
of solution S.
5.3.2.3 Method:
5.3.2.3.1
Take
a test tube add in it 1.0ml of solution S with the help of pipette.
5.3.2.3.2
Acidify
with dilute nitric acid.
5.3.2.3.3
And
add 0.4ml of silver nitrate R1.
5.3.2.3.4
Shake
and allow it to stand.
5.3.2.3.5
A
curdled, white ppt is formed.
5.3.2.3.6
Centrifuge
it in centrifugation machine, according to SOP.
5.3.2.3.7
The
obtained ppt is wash with 3 quantities, each of 1ml, of purified water.
5.3.2.3.8
Carry
out this operation rapidly is subdued light, degrading the fact that the
supernatant solution may not become perfectly clear.
5.3.2.3.9
Suspend
the precipitate in 2.0ml of water and add 1.5ml of ammonia.
5.3.2.3.10 Observe the changes.
5.3.2.4 Observations:
5.3.2.4.1
The
precipitate dissolves easily with the possible exception of a few large
particles which dissolves slowly.
5.4 Assay:
5.4.1
Apparatus:
5.4.1.1 Glassware (according to requirement).
5.4.1.2 Potentiometer.
5.4.1.3 Magnetic stirrer.
5.4.2
Material and reagents:
5.4.2.1 5.0ml of 0.01M hydrochloric acid.
5.4.2.2 50.0ml of ethanol (96%).
5.4.2.3 0.1M sodium hydroxide.
5.4.2.4 Thymolphthalein solution (as indicator).
5.4.3
Sample:
5.4.3.1 0.150g.
5.4.4
Method of analysis:
5.4.4.1 Take a 100.0ml of beaker and take 0.150g of
sample in it.
5.4.4.2 Add 50.0ml of ethanol (96%) and 5.0ml of
0.01M hydrochloric acid dissolve by using magnetic stirrer.
5.4.4.3 Fill the right hand side burette with
titrant 0.1M sodium hydroxide.
5.4.4.4 Carry out a Potentiometric titration using
thymolphthalein solution (as indicator).
5.4.4.5 Operate potentiometer according to SOP.
5.4.4.6 To neutralize analyte add titrant fixed
volume (1ml, 0.5ml or 0.1ml) from burette every time note the reading of change
in potential difference (millivolts) for each addition in given annexure-1.
5.4.4.7 Plot a graph, volume used v/s millivolts.
5.4.4.8 Find out the END POINT. Read the volume
added between the 2 points of inflexion.
5.4.4.9 Peak of graph indicates END POINT i.e. the
point at which maximum millivolts. Note down volume used at that point.
5.4.4.10 Perform blank titration without using
sample. Similarly, as sample titration performed. Record observations in
annexure-1.
5.4.4.11 Calculate volume used by substance by
using formula:
Volume
used by substance = Blank titration - Sample titration.
5.4.4.12 Calculate percentage purity of the sample
by using formula:
%age
purity = volume used by substance x factor x 100
Weight of sample
5.4.5
Factor:
5.4.5.1 1ml of 0.1M sodium hydroxide is equivalent
to 18.77mg of amantadine
hydrochloride C10H18ClN.
5.4.6
Limit:
5.4.6.1 98.5% to 101.0% (anhydrous substance).
6.0 REVISION
LOG:
Revision No.
|
Effective Date
|
Reason
|
00
|
New
SOP
|
7.0 REFERENCES:
7.1 The British Pharmacopoeia. Vol I., Official Monograph / Amantadine hydrochloride: 2015, pp. 127-128.
7.2 The British Pharmacopoeia. Vol V., Official Monograph /Qualitative
Reactions and Tests: 2015, pp. 266-270.
8.0 ANNEXURES:
Annexure 1:
Assay observations and calculations (Potentiometric titration).
Annexure: 1
Assay
observations and calculations (Potentiometric titration)
Potentiometric
titration
Reference
electrode: ___________________
Indicator
electrode: ____________________
Speed
of magnetic stirrer: _______________
Titrant
used: __________________________
Indicator:
____________________________
Blank titration:
Plot
a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT
of blank titration.
Sample
titration:
Plot
a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT
of sample titration:
Volume
used by Blank titration: __________________
Volume
used by Sample titration: _________________
Volume
used by substance = Blank titration - Sample titration.
mV
used by Blank titration: __________________
mV
used by Sample titration: _________________
mV used by substance = Blank titration -
Sample titration.
Volume
used by substance: _______________________
Voltmeter
(mV) used by substance: _________________
RESULT: ____________________________________________________________
|
9.0
ABBREVIATIONS:
Abbreviation
|
Expanded Form
|
SOP
|
Standard
operating procedure
|
&
|
And
|
No.
|
Number
|
Ltd.
|
Limited
|
QCA
|
Quality
control active ingredient
|
F
|
Format
|
Q.C
|
Quality
control
|
Vol
|
Volume
|
v/s
|
Verses
|
mV
|
Millivolts
|
G
|
Grams
|
ml
|
Milliliter
|
Min
|
Minutes
|
oC
|
Degree
centigrade
|
mg
|
Milligram
|
M
|
Molar
|
%
|
Percentage
|
R
|
Reagent
|
g/L
|
Gram
per liter
|
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