MEPYRAMINE MALEATE SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Mepyramine 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 slightly yellowish.
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 very soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is freely soluble.
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.
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 99oC-103oC.
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        0.01M hydrochloric acid.
5.2.2.2  Sample:
5.2.2.2.1        0.1g.
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 0.1g of sample in it.
5.2.2.3.1.2  Dissolve it in sufficient quantity of 0.01M 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 1.0ml of this solution in 100.0ml of beaker.
5.2.2.3.1.5  And dilute it to 100.0ml with 0.01M hydrochloric acid.
5.2.2.3.2        Spectral range:
5.2.2.3.2.1  220-350nm.
5.2.2.3.3        Absorption maxima:
5.2.2.3.3.1  The solution shows 2 absorption maxima 239nm and 316nm.
5.2.2.3.4        Operate the UV/VIS spectrophotometer according to the SOP.
5.2.2.3.5        Measure the absorbance of the resulting solution at the maximum wavelength 239nm and 316nm.
5.2.2.3.6        Note down values of absorbance in annexure-2.
5.2.2.3.7        Calculate the specific absorbances at the absorption maxima by using formula:
1cmA1% = __a__  
               b.c
5.2.2.4  Observations:
5.2.2.4.1        Specific absorbance at 239nm:
5.2.2.4.1.1  431 to 477.
5.2.2.4.2        Specific absorbance at 316nm:
5.2.2.4.2.1  196 to 220.
5.2.3         
5.2.3.1  Material and equipment:
5.2.3.1.1        Glassware (2 test tubes, 1 pipette, 1 spatula).
5.2.3.1.2        Analytical weighing balance.
5.2.3.1.3        Water-bath.
5.2.3.1.4        Vortex mixer.
5.2.3.1.5        Mortar and pestle.
5.2.3.1.6        1.0ml of strong sodium hydroxide solution.
5.2.3.1.7        Ether.
5.2.3.1.8        Resorcinol.
5.2.3.1.9        Sulfuric acid.
5.2.3.1.10    1.0ml of bromine water.
5.2.3.1.11    Purified water.
5.2.3.2  Sample:
5.2.3.2.1        0.1g.
5.2.3.3  Method:
5.2.3.3.1        Take mortar and pestle and add 0.1g of sample in it and add 3.0ml of purified water and 1.0ml of strong sodium hydroxide solution with the help of pipette, and triturate it.
5.2.3.3.2        Take sample in test tube and shake with 3 quantities each of 5.0ml of ether.
5.2.3.3.3        Take 0.1ml of aqueous layer in another test tube A after separating layers.
5.2.3.3.4        Add a solution of 10.0mg of resorcinol in 3.0ml of sulfuric acid.
5.2.3.3.5        Heat it on water-bath for 15min, observe change.
5.2.3.3.6        No colour develops.
5.2.3.3.7        To the rest of the aqueous layer in another test tube B add 1.0ml of bromine water.
5.2.3.3.8        Heat on water-bath for 15min and then heat to boiling and cool it.
5.2.3.3.9        Take 0.2ml of this solution in another test tube C.
5.2.3.3.10    Add a solution of 10.0mg of resorcinol in 3.0ml of sulfuric acid.
5.2.3.3.11    Heat it on water-bath for 15min and observe the changes.
5.2.3.4  Observations:
5.2.3.4.1        A violet-pink colour develops.
5.3  Loss on drying:
5.3.1        Material and equipment:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Analytical weighing balance.
5.3.1.3  Oven.
5.3.2        Sample:
5.3.2.1  1.0g.
5.3.3        Method:
5.3.3.1  Weigh 1.0g of the test sample.
5.3.3.2  Set the oven apparatus. Operate it according to the SOP.
5.3.3.3  Place the sample into the tray and dry it.
5.3.3.4  Set the temperature of oven at 80oC for 45min.
5.3.3.5  And wait till the sample loses its moisture.
5.3.3.6  After 45min weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.7  Note down readings on given Annexure-3.
5.3.4        Observation:
5.3.4.1  Maximum 0.25%.
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  40.0ml 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  0.15g.
5.4.4        Method of analysis:
5.4.4.1  Take a 50.0ml of beaker and take 0.15g of sample in it.
5.4.4.2  Add 40.0ml of anhydrous acetic acid in it and dissolve by using magnetic stirrer i.e. SOP.
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 20.07mg of Mepyramine maleate C21H27N3O5.
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 /Mepyramine maleate: 2015, pp. 217-218.
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 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
Observations and Calculations of UV/VIS spectrophotometer
UV/VIS spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
Thickness of cell:

Spectral range:
220-350nm.
Maxima absorption wavelength:
239nm and 316nm.
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 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
mg
Milligram
ml
Milliliter
ppt
Precipitate
M
Molar
g
Grams
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
Hrs.
Hours
A
Absorbance


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