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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