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:
Average: _______________
Optical
rotation of blank solution: _______________
Sample solution:
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=
_________________
Average
% 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:
Plot
a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT
of blank titration.
Sample
titration:
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
|
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