CHLORHEXIDINE GLUCONATE

CHLORHEXIDINE GLUCONATE

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 105^oC.

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 132^oC to 136^oC.

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