DOMPERIDONE MALEATE SOP


DOMPERIDONE MALEATE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Domperidone 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 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        Dimethylformamide.
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 Dimethylformamide 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 Ethanol (96%) 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 slightly soluble.
5.1.2.4.2        The sample in test tube 2 containing with Dimethylformamide is sparingly soluble.
5.1.2.4.3        The sample in test tube 3 containing with Methanol is slightly soluble.
5.1.2.4.4        The sample in test tube 4 containing with ethanol (96%) very slightly soluble.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (2 test tubes, 1 pipette, 1 spatula).
5.2.1.1.2        Analytical weighing balance.
5.2.1.1.3        Water-bath.
5.2.1.1.4        Vortex mixer.
5.2.1.1.5        Mortar and pestle.
5.2.1.1.6        1.0ml of strong sodium hydroxide solution.
5.2.1.1.7        Ether.
5.2.1.1.8        Resorcinol.
5.2.1.1.9        Sulfuric acid.
5.2.1.1.10    2.0ml of bromine water.
5.2.1.1.11    Purified water.
5.2.1.2  Sample:
5.2.1.2.1        0.1g.
5.2.1.3  Method:
5.2.1.3.1        Take mortar and pestle and add 0.1g of sample in it and add a mixture of 1.0ml of strong sodium hydroxide solution and 3.0ml of purified water with the help of pipette, and triturate it.
5.2.1.3.2        Take sample in test tube and shake with 3 quantities each of 5.0ml of ether.
5.2.1.3.3        Take 0.1ml of aqueous layer in another test tube A after separating layers.
5.2.1.3.4        Add a solution of 10.0mg of resorcinol in 3.0ml of sulfuric acid.
5.2.1.3.5        Heat it on water-bath for 15min, observe change.
5.2.1.3.6        No colour develops.
5.2.1.3.7        To the rest of the aqueous layer in another test tube B add 2.0ml of bromine solution.
5.2.1.3.8        Heat on water-bath for 15min and then heat to boiling and cool it.
5.2.1.3.9        Take 0.1ml of this solution in another test tube C.
5.2.1.3.10    Add a solution of 10.0mg of resorcinol in 3.0ml of sulfuric acid.
5.2.1.3.11    Heat it on water-bath for 15min and observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        A violet 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 105oC 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-1.
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  Titration apparatus.
5.4.1.3  Water-bath.
5.4.2        Material and reagents:
5.4.2.1  50.0ml of anhydrous acetic acid.
5.4.2.2  0.2ml of naphtholbenzein solution (as indicator).
5.4.2.3  0.1M perchloric acid.
5.4.3        Sample:
5.4.3.1  0.4g.
5.4.4        Method of analysis:
5.4.4.1  Sample titration:
5.4.4.1.1        Take a flask and add in it 0.4g of sample.
5.4.4.1.2        Dissolve it in 50.0ml of anhydrous acetic acid.
5.4.4.1.3        Set titration apparatus.
5.4.4.1.4        Use 0.2ml of naphtholbenzein solution as indicator.
5.4.4.1.5        Titrate with 0.1M perchloric acid, until the colour is changes from orange-yellow to green.
5.4.4.1.6        Note down the volume used as shown in Annexure-2.
5.4.4.1.7        Take at least 3 readings and take average.
5.4.4.2  Blank titration:
5.4.4.2.1        Take a flask and add in it 50.0ml of anhydrous acetic acid.
5.4.4.2.2        Set titration apparatus.
5.4.4.2.3        Use 0.2ml of naphtholbenzein solution as indicator.
5.4.4.2.4        Titrate with 0.1M perchloric acid, until the colour is changes from orange-yellow to green.
5.4.4.2.5        Note down the volume used as shown in Annexure-2.
5.4.4.2.6        Take at least 3 readings and take average.
5.4.4.3  Calculate percentage purity.
5.4.4.4  Calculations:
5.4.4.4.1        After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                               Weight of sample
5.4.4.4.3        Put values and calculate %age purity.
5.4.5        Factor:
5.4.5.1  1ml of 0.1M perchloric acid is equivalent to 54.20mg of Domperidone maleate C26H28ClN5O6.
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 I., Official Monograph / Domperidone Maleate: 2015, pp. 804-806.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using oven.
Annexure 2: Observations and calculations of assay.


Annexure: 1
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: 2
Observations and calculations assay
Indicator: ___________________
Weight of sample: ____________                                                Factor: ______________
Titrant: _____________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Calculations:
Volume used by substance = Blank titration - Sample titration.

%age purity = volume used by substance x factor x 100
                                                                     Weight of sample

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
R
Reagent
oC
Degree centigrade
vi
Initial volume
vf
Final volume


No comments:

Post a Comment