CHLORPHENAMINE MALEATE SOP


CHLORPHENAMINE MALEATE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Chlorphenamine maleate 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 containing with purified water is freely soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is 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  Purified water.
5.2.2        Sample:
5.2.2.1  2.0g.
5.2.3        Preparation of solution S:
5.2.3.1  Take a beaker of 50.0ml and add sample 2.0g in it.
5.2.3.2  Add in it sufficient quantity of purified water.
5.2.3.3  Dilute it to 20.0ml with the same solvent.
5.3  Identification tests:
5.3.1        Melting point determination:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        Melting point apparatus.
5.3.1.1.3        Capillary tubes.
5.3.1.1.4        Purified water.
5.3.1.2  Sample:
5.3.1.2.1        Sufficient quantity of sample.
5.3.1.3  Method:
5.3.1.3.1        Introduce the sufficient quantity of sample into a capillary tube.
5.3.1.3.2        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the centre of the bulb of thermometer.
5.3.1.3.3        Switch on the melting point apparatus.
5.3.1.3.4        Operate the melting point apparatus
5.3.1.3.5        Raise the temperature of the apparatus.
5.3.1.3.6        Record the temperature at which the last particle passes into the liquid phase.
5.3.1.3.7        Record measurements in annexure-1.
5.3.1.4  Observations:
5.3.1.4.1        The melting point is 130oC-135oC.
5.3.2        Optical rotation:
5.3.2.1  Material and equipment:
5.3.2.1.1        Polarimeter.
5.3.2.1.2        Analytical weighing balance.
5.3.2.1.3        Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula, 1 glass rod).
5.3.2.1.4        Purified water.
5.3.2.2  Sample:
5.3.2.2.1        Solution S.
5.3.2.3  Method:
5.3.2.3.1        Firstly clean the Polarimeter with clean dry cloth,
5.3.2.3.2        Operate the Polarimeter
5.3.2.3.3        Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.3.2.3.4        Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.3.2.3.5        Note down the values in annexure-2.
5.3.2.4  Observations:
5.3.2.4.1        -0.10o to +0.10o.
5.4  Loss on drying:
5.4.1        Material and equipment:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Analytical weighing balance.
5.4.1.3  Oven.
5.4.2        Sample:
5.4.2.1  1.0g.
5.4.3        Method:
5.4.3.1  Weigh 1.0g of the test sample.
5.4.3.2  Set the oven apparatus.
5.4.3.3  Place the sample into the tray and dry it.
5.4.3.4  Set the temperature of oven at 105oC for 4h.
5.4.3.5  And wait till the sample loses its moisture.
5.4.3.6  After 4h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.4.3.7  Note down readings on given Annexure-3.
5.4.4        Observation:
5.4.4.1  Maximum 0.5%.
5.5  Assay:
5.5.1        Apparatus:
5.5.1.1  Glassware (according to requirement).
5.5.1.2  Potentiometer.
5.5.1.3  Magnetic stirrer.
5.5.2        Material and reagents:
5.5.2.1  25.0ml of anhydrous acetic acid.
5.5.2.2  0.1M Perchloric acid.
5.5.2.3  Crystal violet solution (as an indicator).
5.5.3        Sample:
5.5.3.1  0.15g.
5.5.4        Method of analysis:
5.5.4.1  Take a 50.0ml of beaker and take 0.15g of sample in it.
5.5.4.2  Add 25.0ml of anhydrous acetic acid in it and dissolve by using magnetic stirrer operate.
5.5.4.3  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.5.4.4  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.5.4.5  Operate potentiometer
5.5.4.6  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-4.
5.5.4.7  Plot a graph, volume used v/s millivolts.
5.5.4.8  Find out the END POINT.
5.5.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.5.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-4.
5.5.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.5.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                         Weight of sample
5.5.5        Factor:
5.5.5.1  1ml of 0.1M Perchloric acid is equivalent to 19.54mg of Chlorphenamine maleate C20H23ClN2O4.
5.5.6        Limit:
5.5.6.1  98.0% to 101.0% (dried 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 / Chlorphenamine maleate: 2015, pp. 524-525.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Optical rotation observations and calculations.
Annexure 3: Observations of Percentage Loss of drying by using oven.
Annexure 4: Assay observations and calculations (Potentiometric titration).



Annexure: 1
Observations of Melting point apparatus
Sample = _____________
Time period = _____________
Sr.#
Initial (Ti)
(oC)
Final (Tf)
(oC)
Tf - Ti
(oC)












Average: _____________

Result: _________________

Remarks: _______________________________________________________________













Annexure: 2
Optical rotation observations and calculations
Optical rotation
Instrument: ___________________                                              Date: _______________
Model: _______________________        Length of Polarimeter tube: ________________
Sample: ________________________________g.
Solvent: ________________________________ml.
Concentration of sample solution: ____________g/ml.
Blank solution:
Sr.#
Blank solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of blank solution: _______________
Sample solution:
Sr.#
Sample solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of sample solution: ______________
Optical rotation of substance = Blank solution - Sample solution.








                                                                      Result: ________________
Remarks: ___________________________________________________________



















Annexure: 3
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
Apparatus: ___________________
Temperature: __________________
Weight of Sample = _____________
Time period = _____________
Pressure= _________________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:






Remarks: _______________________________________________________________




Annexure: 4
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
BP
British Pharmacopoeia
mg
Milligram
ml
Milliliter
M
Molar
g
Grams
Min
Minute
%
Percentage
v/s
Verses
mV
Millivolts
oC
Degree centigrade
h
Hours
Ti
Initial temperature
Tf
Final temperature
Temp.
Temperature
o
Degree (angle)
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
λ
Lambda
g/L
Grams per liter


No comments:

Post a Comment