LOSARTAN POTASSIUM SOP
1.0 OBJECTIVE:
To
lay down a procedure of analytical report for the active raw material of the Losartan Potassium 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.
5.1.1.3
Hygroscopic.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (test
tubes, spatula).
5.1.2.1.2
Methanol.
5.1.2.1.3
Acetonitrile.
5.1.2.1.4
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 3 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 methanol in
test tube 2 and observe.
5.1.2.3.4
Add acetonitrile
in test tube 3 and observe.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with water is freely soluble.
5.1.2.4.2
The sample in test
tube 2 containing with methanol is freely soluble.
5.1.2.4.3
The sample in test
tube 3 containing with acetonitrile is slightly soluble.
5.2 Identification
tests:
5.2.1
Potassium
test:
5.2.1.1
Material and equipment:
5.2.1.1.1
Glassware
(according to requirement).
5.2.1.1.2
Water bath.
5.2.1.1.3
Sodium carbonate
solution
5.2.1.1.4
Sodium sulfide
solution.
5.2.1.1.5
Ice-water.
5.2.1.1.6
150g/L solution of
tartaric acid.
5.2.1.1.7
Purified water.
5.2.1.2
Sample:
5.2.1.2.1
25.0mg.
5.2.1.3
Method:
5.2.1.3.1
Take a test tube
and add 25.0mg of sample in it.
5.2.1.3.2
Dissolve it in
3.0ml of purified water.
5.2.1.3.3
Take 2.0ml of this
solution in another test tube.
5.2.1.3.4
Add 1.0ml of
sodium carbonate solution and heat it on water bath.
5.2.1.3.5
Observe the
changes. There is no ppt formed.
5.2.1.3.6
Add to this hot
solution 0.05ml of sodium sulfide solution.
5.2.1.3.7
Again observe the
changes. There is no ppt formed.
5.2.1.3.8
Take a beaker
half-full iced-water and cool the test tube in it. And add 2.0ml of a 150g/L
solution of tartaric acid.
5.2.1.3.9
Allow it to stand.
5.2.1.3.10 Observe
the changes.
5.2.1.4
Observations:
5.2.1.4.1
A white
crystalline ppt is formed.
5.3 Assay:
5.3.1
Apparatus:
5.3.1.1
Glassware
(according to requirement).
5.3.1.2
Potentiometer.
5.3.2
Material
and reagents:
5.3.2.1
Anhydrous acetic
acid.
5.3.2.2
0.1M Perchloric
acid.
5.3.2.3
Crystal violet solution.
5.3.3
Sample:
5.3.3.1
0.200g.
5.3.4
Method
of analysis:
5.3.4.1 Take
a 50.0ml of beaker and take 0.200g of sample in it.
5.3.4.2 Add
75.0ml of anhydrous acetic acid in it and sonicate for 10min.
5.3.4.3 Fill
the right hand side burette with titrant 0.1M Perchloric acid.
5.3.4.4 Carry
out a Potentiometric titration using crystal violet solution as an indicator.
5.3.4.5 Operate
potentiometer according to SOP.
5.3.4.6 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.
5.3.4.7 Plot
a graph, volume used v/s millivolts.
5.3.4.8 Find
out the END POINT.
5.3.4.9 Peak
of graph indicates END POINT i.e. the point at which maximum millivolts. Note
down volume used at that point.
5.3.4.10 Perform
blank titration without using sample. Similarly, as sample titration performed.
Record observations in annexure-1.
5.3.4.11 Calculate
volume used by substance by using formula:
Volume
used by substance = Blank titration - Sample titration.
5.3.4.12 Calculate
percentage purity of the sample by using formula:
%age
purity = volume used by substance x factor x 100
Weight of sample
5.3.5
Factor:
5.3.5.1 1ml
of 0.1M Perchloric acid is equivalent to 23.05mg of Losartan Potassium C22H22ClKN6O.
5.3.6
Limit:
5.3.6.1
98.5% to 101.5%
(dried substance).
6.0 REVISION LOG:
|
Revision No.
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Effective Date
|
Reason
|
|
00
|
|
New SOP
|
7.0 REFERENCES:
7.1
The British
Pharmacopoeia. Vol II.,
Official Monograph /Losartan Potassium: 2015, pp. 136-138.
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: ____________________________________________________________
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9.0 ABBREVIATIONS:
|
Abbreviation
|
Expanded Form
|
|
SOP
|
Standard
operating procedure
|
|
&
|
And
|
|
No.
|
Number
|
|
Ltd.
|
Limited
|
|
Q.C
|
Quality
control
|
|
B.P
|
British
pharmacopoeia
|
|
g/L
|
Grams
per liter
|
|
mg
|
Milligram
|
|
ml
|
Milliliter
|
|
ppt
|
Precipitate
|
|
M
|
Molar
|
|
g
|
Grams
|
|
Min
|
Minute
|
|
%
|
Percentage
|
|
Vol
|
Volume
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|