CETRIMIDE SOP



CETRIMIDE SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Cetrimide from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
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  Voluminous.
5.1.1.3  Free-flowing powder.
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        Purified water.
5.1.2.1.3        (alcohol) Ethanol (96%).
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 it.
5.1.2.3.3        Add alcohol in test tube 2 and observe it.
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 alcohol is also freely soluble.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Alcohol.
5.2.1.1.3        U.V spectrophotometer.
5.2.1.2  Sample:
5.2.1.2.1        0.25g.
5.2.1.3  Method of analysis:
5.2.1.3.1        Take a 50ml beaker and dissolve in it 0.25g of sample in small amount of alcohol.
5.2.1.3.2        And dilute to 25.0ml with the same solvent.
5.2.1.3.3        According to SOP of UV/visible spectrophotometer operate i.e and observe the absorbance of solution at wavelength 260nm to 280nm.
5.2.1.4  Observation:
5.2.1.4.1        The absorbance of the solution has a maximum of 0.05.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Buffer solution pH 8.0
5.2.2.1.3        Potassium ferricyanide.
5.2.2.2  Sample:
5.2.2.2.1        5.0mg.
5.2.2.3  Method of analysis:
5.2.2.3.1        Sample solution:
5.2.2.3.1.1  Take a test tube and dissolve about 5.0mg of the sample in 5ml of buffer solution pH 8.0.
5.2.2.3.1.2  Add about 10.0mg of potassium ferricyanide.
5.2.2.3.1.3  And observe the changes.
5.2.2.3.2        Blank solution:
5.2.2.3.2.1  Take a test tube and take in it 5ml of buffer solution pH 8.0.
5.2.2.3.2.2  Add about 10.0mg of potassium ferricyanide.
5.2.2.3.2.3  And observe the changes.
5.2.2.4  Observation:
5.2.2.4.1        Sample solution:
5.2.2.4.1.1  A yellow ppt is formed.
5.2.2.4.2        Blank solution:
5.2.2.4.2.1  A yellow solution is observed but no ppt is formed.
5.2.3         
5.2.3.1  Material and equipment:
5.2.3.1.1        Glassware (according to requirement).
5.2.3.1.2        Carbon dioxide-free water.
5.2.3.2  Sample:
5.2.3.2.1        2.0g.
5.2.3.3  Method:
5.2.3.3.1        Solution S:
5.2.3.3.1.1  Take a beaker of 100ml and dissolve 2.0g of sample in carbon dioxide-free water.
5.2.3.3.1.2  And dilute to 100ml with the same solvent.
5.2.3.3.2        Take a test tube and half-fill it with the Solution S.
5.2.3.3.3        And shake it well.
5.2.3.4  Observation:
5.2.3.4.1        Solution S froths copiously when shaken.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Separating funnel.
5.3.2        Sample:
5.3.2.1  2.0g.
5.3.3        Material and reagents:
5.3.3.1  Chloroform.
5.3.3.2  Purified water.
5.3.3.3  0.1M sodium hydroxide.
5.3.3.4  50g/L solution of potassium iodide.
5.3.3.5  Hydrochloric acid.
5.3.3.6  0.05M potassium iodate.
5.3.4        Method of analysis:
5.3.4.1  Solution:
5.3.4.1.1        Firstly prepare the solution, take a 100ml of beaker.
5.3.4.1.2        Dissolve 2.0g of sample in water.
5.3.4.1.3        And dilute to 100ml with the same solvent.
5.3.4.2  Take a separating funnel transfer 25.0ml of solution, 25.0ml of chloroform, 10.0ml of 0.1M NaOH and 10.0ml of freshly prepared 50g/L solution of potassium iodide.
5.3.4.3  Shake it well.
5.3.4.4  Allow it to separate the layers (aqueous layer and chloroform layer).
5.3.4.5  Discard the chloroform layer.
5.3.4.6  Divide the aqueous layer into 3 quantities.
5.3.4.7  In each 3 quantities of aqueous layer add 10ml of chloroform.
5.3.4.8  And shake it well again in separating funnel.
5.3.4.9  Allow it to separate the layers (aqueous layer and chloroform layer).
5.3.4.10       Discard the chloroform layer.
5.3.4.11       Take aqueous layer, add 40ml of hydrochloric acid and allow it to cool.
5.3.4.12       Set the titration apparatus.
5.3.4.13       Titrate it with 0.05M potassium iodate until the deep brown colour is almost discharged.
5.3.4.14       Add 2ml of chloroform and continue the titration, shaking vigorously, until the colour of the chloroform layer no longer changes.
5.3.4.15    Blank titration:
5.3.4.15.1    Carry out a blank titration.
5.3.4.15.2    Take conical flask and add in it a mixture of 10.0ml of the freshly prepared 50g/L solution of potassium iodide, 20ml of water and 40ml of hydrochloric acid.
5.3.4.15.3    Titrate it with 0.05M potassium iodate.
5.3.5        Calculations:
5.3.5.1  After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.5.2  For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                         Weight of sample
5.3.5.3  Put values and calculate %age purity.
5.3.6        Factor:
5.3.6.1  1ml of 0.05M potassium iodate is equivalent to 33.64mg of C17H38BrN.
5.3.7        Limit:
5.3.7.1  96.0% to 101.0%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Cetrimide: 2015, pp. 491-492.
8.0  ANNEXURES:
8.1  Not Applicable.


9.0  ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
Q.C
Quality control
B.P
British pharmacopoeia
%
Percentage
U.V
Ultraviolet
g
Gram
ml
Milliliter
nm
Nanometer
ppt
Precipitate
M
Molar
g/L
Gram per liter
NaOH
Sodium hydroxide
QCA
Quality control active ingredient
F
Format


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