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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.
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:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of blank titration.
Sample titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












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
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


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