MEBEVERINE HYDROCHLORIDE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Mebeverine Hydrochloride 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 (3 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Ether.
5.1.2.1.4        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 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 Ethanol (96%) in test tube 2 and observe.
5.1.2.3.4        Add ether in test tube 3 and observe
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1containing with purified water is very soluble.
5.1.2.4.2        The sample in test tube 2 containing with Ethanol (96%) is freely soluble.
5.1.2.4.3        The sample in test tube 2 containing with ether is practically insoluble.
5.2  Identification tests:
5.2.1        Chlorides test:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (test tube, spatula, beaker, glass rod).
5.2.1.1.2        Centrifugation machine.
5.2.1.1.3        2M nitric acid.
5.2.1.1.4        Purified water.
5.2.1.1.5        0.4ml of Silver nitrate R1.
5.2.1.1.6        Ammonia.
5.2.1.2  Sample:
5.2.1.2.1        25.0mg.
5.2.1.3  Method:
5.2.1.3.1        Take a test tube add in it 2.0ml of water with the help of pipette.
5.2.1.3.2        Add 25.0mg of sample and dissolve it.
5.2.1.3.3        Acidify it with 2M nitric acid.
5.2.1.3.4        Centrifuge it in centrifugation machine, according to SOP.
5.2.1.3.5        The supernatant liquid is produced; add 0.4ml of silver nitrate solution R1 in it.
5.2.1.3.6        Shake and allow it to stand.
5.2.1.3.7        A curdled, white ppt is formed.
5.2.1.3.8        Centrifuge it again in centrifugation machine, according to SOP.
5.2.1.3.9        The obtained ppt is wash with 3 quantities, each of 1ml, of water.
5.2.1.3.10    Carry out this operation rapidly is subdued light, degrading the fact that the supernatant solution may not become perfectly clear.
5.2.1.3.11    Suspend the precipitate in 2.0ml of water and add 1.5ml of ammonia
5.2.1.4  Observations:
5.2.1.4.1        The precipitate dissolves easily with the possible exception of a few large particles which dissolves slowly.
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 105oC for at least 1 hour.
5.3.3.5  And wait till the sample loses its moisture.
5.3.3.6  After 1 hour weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.7  Note down readings on given Annexure-1.
5.3.4        Observation:
5.3.4.1  Loses not more than 0.5% of its weight.
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  7.0ml of mercury (II) acetate solution.
5.4.2.2  0.1M Perchloric acid.
5.4.3        Sample:
5.4.3.1  0.4g.
5.4.4        Method of analysis:
5.4.4.1  Take a 50.0ml of beaker and add 0.4g of sample in it.
5.4.4.2  And add 7.0ml of mercury (II) acetate solution.
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.
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-2.
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-2.
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  Each ml of 0.1M Perchloric acid VS is equivalent to 46.60mg of Mebeverine hydrochloride C25H35NO5.HCl.
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 / Mebeverine hydrochloride: 2015, pp. 194-195.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using oven.
Annexure 2: Assay observations and calculations (Potentiometric titration).


Annexure: 1
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
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: 2
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
FOormat
Q.C
Quality control
Vol
Volume
%
Percentage
g
Grams
ml
Milliliter
M
Molar
g/L
Grams per liter
mg
Milligram
B.P
British pharmacopoeia
oC
Degree centigrade
R
Reagent
v/s
Verses
mV
Millivolts
H
Hours


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