AMANTADINE HYDROCHLORIDE SOP


AMANTADINE HYDROCHLORIDE SOP

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:
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
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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