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PHENIRAMINE MALEATE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Pheniramine 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 (4 test tubes, 1 spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Purified water.
5.1.2.1.4        Methanol.
5.1.2.1.5        Methylene chloride.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 4 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.
5.1.2.3.4        Add Methanol in test tube 3 and observe.
5.1.2.3.5        Add Methylene chloride in test tube 4 and observe
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is very soluble.
5.1.2.4.2        The sample in test tube 2, 3 & 4 containing with ethanol (96%), methanol and methylene chloride is freely soluble respectively.
5.2  Identification tests:
5.2.1        Melting point determination:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Melting point apparatus.
5.2.1.1.3        Capillary tubes.
5.2.1.1.4        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        Sufficient quantity of sample.
5.2.1.3  Method:
5.2.1.3.1        Introduce the sufficient quantity of sample into a capillary tube.
5.2.1.3.2        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.
5.2.1.3.3        Switch on the melting point apparatus.
5.2.1.3.4        Operate the melting point apparatus according to the SOP No. BM/QCEO/SOP009-00.
5.2.1.3.5        Raise the temperature of the apparatus.
5.2.1.3.6        Record the temperature at which the last particle passes into the liquid phase.
5.2.1.3.7        Record measurements in annexure-1.
5.2.1.4  Observations:
5.2.1.4.1        The melting point is 106oC-109oC.
5.2.2        UV/VIS absorption Spectrophotometry:
5.2.2.1  Material and equipment:
5.2.2.1.1        UV/VIS Spectrophotometer.
5.2.2.1.2        Glassware (according to requirement).
5.2.2.1.3        0.1M hydrochloric acid.
5.2.2.2  Sample:
5.2.2.2.1        40.0mg.
5.2.2.3  Method:
5.2.2.3.1        Test solution:
5.2.2.3.1.1  Take a beaker of 100.0ml and add 40.0mg of sample in it.
5.2.2.3.1.2  Dissolve it in sufficient quantity of 0.1M hydrochloric acid.
5.2.2.3.1.3  And dilute it to 100.0ml with the same acid.
5.2.2.3.1.4  Take 5.0ml of this solution in 50.0ml of beaker.
5.2.2.3.1.5  And dilute it to 50.0ml with 0.1M hydrochloric acid.
5.2.2.3.2        Spectral range:
5.2.2.3.2.1  220-320nm.
5.2.2.3.3        Absorption maximum:
5.2.2.3.3.1  At 265nm.
5.2.2.3.4        Shoulder:
5.2.2.3.4.1  At 261nm.
5.2.2.3.5        Operate the UV/VIS spectrophotometer according to the SOP No. BM/QCEO/SOP027-00.
5.2.2.3.6        Measure the absorbance of the resulting solution at the maximum wavelength 265nm.
5.2.2.3.7        Note down values of absorbance in annexure-2.
5.2.2.3.8        Calculate the specific absorbances at the absorption maximum by using formula:
1cmA1% = __a__  
                    b.c
5.2.2.4  Observations:
5.2.2.4.1        Specific absorbance at absorption maximum:
5.2.2.4.1.1  200 to 220.
5.3  Loss on drying:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        Desiccator.
5.3.1.1.3        Diphosphorous pentaoxide.
5.3.1.1.4        Analytical weighing balance.
5.3.1.1.5        Spatula.
5.3.1.2  Sample:
5.3.1.2.1        1.0g.
5.3.1.3  Method:
5.3.1.3.1        Weigh 1g of the test sample.
5.3.1.3.2        Set the desiccator apparatus with desiccant.
5.3.1.3.3        Operate the desiccator according to the SOP.
5.3.1.3.4        Place the sample into the china dish or petri dish.
5.3.1.3.5        Set the temperature 60oC and at 1.5kPa to 2.5kPa pressure for at least 3h.
5.3.1.3.6        And wait till the sample loses its moisture.
5.3.1.3.7        After 3h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.1.3.8        Note down readings on given Annexure-3.
5.3.1.4  Observations:
5.3.1.4.1        Maximum 0.5%.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Potentiometer.
5.4.1.3  Magnetic stirrer.
5.4.2        Material and reagents:
5.4.2.1  50.0ml of anhydrous acetic acid.
5.4.2.2  0.1M Perchloric acid.
5.4.2.3  Crystal violet solution.
5.4.3        Sample:
5.4.3.1  0.13g.
5.4.4        Method of analysis:
5.4.4.1  Take a 50.0ml of beaker and take 0.13g of sample in it.
5.4.4.2  Add 50.0ml of anhydrous acetic acid in it and dissolve by using magnetic stirrer.
5.4.4.3  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.4.4.4  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.4.4.5  Operate potentiometer according to SOP.
5.4.4.6  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.
5.4.4.7  Plot a graph, volume used v/s millivolts.
5.4.4.8  Find out the END POINT.
5.4.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.4.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-4.
5.4.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
Weight of sample
5.4.5        Factor:
5.4.5.1  1ml of 0.1M Perchloric acid is equivalent to 17.82mg of Pheniramine maleate C20H24N2O4.
5.4.6        Limit:
5.4.6.1  99.0% 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 II., Official Monograph /Pheniramine maleate: 2015, pp. 540-541.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Observations of UV/VIS spectrophotometer.
Annexure 3: Observations of percentage loss of drying.
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
Observations and Calculations of UV/VIS spectrophotometer
UV/VIS spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
Thickness of cell:

Spectral range:
220-320nm.
Maxima absorption wavelength:
265nm.
Sample:

Other reagent used:


No. of obs.
Concentration
(c)
Wavelength
(λ)
Absorbance
(a)
Specific absorbance
A (1%,1cm)











CALCULATIONS:
1cmA1% =  __a__
                   b.c




Results: _______________
Remarks: ______________________________________________________________



Annexure: 3
Observations of percentage loss of drying
Percentage loss of drying
Apparatus: ____________________
Temperature: __________________
Pressure: _____________________
Weight of Sample = _____________
Time period = _____________
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
mg
Milligram
ml
Milliliter
ppt
Precipitate
M
Molar
g
Grams
Cm
Centimeter
Min
Minute
%
Percentage
Ti
Initial temperature
Tf
Final temperature
Temp.
Temperature
v/s
Verses
mV
Millivolts
oC
Degree centigrade
R
Reagent
λ
Lambda
UV/VIS
Ultraviolet/ visible
nm
Nanometer
h
Hours
A
Absorbance
BP
British Pharmacopoeia


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