1.0 OBJECTIVE:
To
lay down a procedure of analytical report for the active raw material of the
Chlorhexidine gluconate solution 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 Manger.
5.0 PROCEDURE:
5.1 Characters:
5.1.1
Appearance:
5.1.1.1 Almost colorless.
5.1.1.2 Pale yellowish liquid.
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
Acetone.
5.1.2.1.4
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
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
acetone with NMT 3 parts, in test tube 2 and observe.
5.1.2.3.4
Add
ethanol (96%) with NMT 5 parts, 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 miscible.
5.1.2.4.2
The
sample in test tube 2 containing with NMT 3 parts of acetone is miscible.
5.1.2.4.3
The
sample in test tube 3 containing with NMT 5 parts of ethanol (96%) is also miscible.
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
Titan
yellow paper strips
5.2.1.1.3
Purified
water.
5.2.1.1.4
Ice
water.
5.2.1.1.5
Strong
sodium hydroxide solution.
5.2.1.1.6
Ethanol
(70% v/v).
5.2.1.1.7
Desiccator.
5.2.1.1.8
Melting
point apparatus (beaker, stirrer, thermometer, capillary tube, burner, thread).
5.2.1.2 Sample:
5.2.1.2.1
1.0
ml.
5.2.1.3 Method of analysis:
5.2.1.3.1
Take
1ml of sample in the 50ml of beaker and add 40ml of water in it.
5.2.1.3.2
Cool
it in ice water, which is present in a 1000ml of beaker half-filled.
5.2.1.3.3
Make
alkaline to titan yellow paper by adding drop wise and with stirring, strong
NaOH solution and add 1ml in excess.
5.2.1.3.4
Filter
it.
5.2.1.3.5
Wash
the ppt with water until the washings are free from alkali and recrystallize
from ethanol (70% v/v).
5.2.1.3.6
Dry
it in desiccator at 100 to 105oC.
5.2.1.3.7
Upon
dry residue perform melting point test.
5.2.1.3.8
Melting
point determination method:
5.2.1.3.8.1 Firstly set the apparatus.
5.2.1.3.8.2 Fill 100ml beaker with water and place
wire gauze on tripod stand, put beaker on it.
5.2.1.3.8.3 Heat up the capillary tube on burner from
center such that it divides into two by pulling the capillary tube from both
sides in opposite directions.
5.2.1.3.8.4 Introduce a sufficient quantity into a
capillary tube to give a compact column 4mm to 6mm in height.
5.2.1.3.8.5 Tie up the capillary tube near the
thermometer bulb with the help of thread.
5.2.1.3.8.6 And hang the thermometer on stand such
that the capillary tube is not fully immersed in water. The immersion mark of
which is at the level of the surface of the liquid.
5.2.1.3.8.7 Allow the burner to heat up the liquid in
beaker.
5.2.1.3.8.8 Observe it closely.
5.2.1.3.8.9 Record the temperature at which the last
particle passes into the liquid phase.
5.2.1.4 Observations:
5.2.1.4.1
The
residue melts at 132oC to 136oC.
5.2.2
5.2.2.1 Material and equipment:
5.2.2.1.1
Glassware
(according to requirement).
5.2.2.1.2
10g/L
solution of cetrimide.
5.2.2.1.3
Strong
sodium hydroxide solution.
5.2.2.1.4
Bromine
water.
5.2.2.2 Sample:
5.2.2.2.1
0.05
ml.
5.2.2.3 Method of analysis:
5.2.2.3.1
Take
a test tube and add in it 0.05ml of sample.
5.2.2.3.2
Add
5ml of a 10g/L solution of cetrimide.
5.2.2.3.3
And
also add 1ml of strong NaOH and 1ml of bromine water.
5.2.2.3.4
Observe
the change in colour.
5.2.2.4 Observations:
5.2.2.4.1
A
deep red colour is produced.
5.3 Assay:
5.3.1
Apparatus:
5.3.1.1 Hydrometer.
5.3.1.2 Potentiometric titration.
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 (as an indicator).
5.3.3
Sample:
5.3.3.1 1.0g.
5.3.4
Method of analysis:
5.3.4.1 Determine the density of the preparation
to be examined by using the hydrometer.
5.3.4.2 Transfer 1.0g to a 250ml of the beaker.
5.3.4.3 And add 50ml of anhydrous acetic acid.
5.3.4.4 Titrate it with 0.1M Perchloric acid.
5.3.4.5 Use crystal violet solution as an
indicator. (prepare it according to B.P Specifications)
5.3.4.6 Determine the end-point
potentiometrically.
5.3.5
Factor:
5.3.5.1 1ml of 0.1M Perchloric acid is equivalent
to 22.44mg of C34H54Cl2N10O14.
5.3.6
Limit:
5.3.6.1 190.0g/L to 210.0g/L.
6.0 REFERENCES:
6.1 The British Pharmacopoeia. Vol I., Official Monograph /Chlorhexidine
gluconate solution: 2015, pp. 510-513.
7.0 ANNEXURES:
7.1 Not Applicable.
8.0 ABBREVIATIONS:
Abbreviation
|
Expanded Form
|
SOP
|
Standard
operating procedure
|
&
|
And
|
No.
|
Number
|
Ltd.
|
Limited
|
Q.C
|
Quality
control
|
%
|
Percentage
|
B.P
|
British
pharmacopoeia
|
NMT
|
Not
more than
|
v/v
|
Volume
by volume
|
ml
|
Milliliter
|
NaOH
|
Sodium
hydroxide
|
oC
|
Degree
centigrade
|
mm
|
Millimeter
|
g/L
|
Gram
per liter
|
g
|
Gram
|
M
|
Molar
|
mg
|
Milligram
|
QCA
|
Quality
control active ingredient
|
F
|
Format
|