DOMPERIDONE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Domperidone from the Pharmacopoeia 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 Ethanol (96%) in test tube 3 and observe.
5.1.2.3.5        Add methanol 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 practically insoluble.
5.1.2.4.2        The sample in test tube 2 containing with Dimethylformamide is soluble.
5.1.2.4.3        The sample in test tube 3 & 4 containing with ethanol (96%) and Methanol is slightly 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 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 244oC-248oC.
5.2.2        Non-nitrogen substituted barbiturates:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (2 test tubes, 1 pipette, 1 spatula).
5.2.2.1.2        Analytical weighing balance.
5.2.2.1.3        3.0ml of methanol.
5.2.2.1.4        100.0g/L solution of cobalt nitrate.
5.2.2.1.5        100.0g/L solution of calcium chloride.
5.2.2.1.6        0.1ml of dilute sodium hydroxide solution.
5.2.2.2  Sample:
5.2.2.2.1        5.0mg.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube and dissolve 5.0mg of the substance to be examined in 3.0ml of methanol.
5.2.2.3.2        And then add 0.1ml of a solution containing 100.0g/L solution of cobalt nitrate and 100.0g/L solution of calcium chloride.
5.2.2.3.3        Mix it and add, with shaking 0.1ml of dilute sodium hydroxide solution.
5.2.2.3.4        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        A violet-blue colour and ppt are formed.
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 No. BM/QCEO/SOP035-00.
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-2.
5.3.4        Observation:
5.3.4.1  Maximum 0.5%.
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  Anhydrous acetic acid.
5.4.2.2  Methyl ethyl ketone.
5.4.2.3  0.2ml of naphtholbenzein solution (as indicator).
5.4.2.4  0.1M perchloric acid.
5.4.3        Sample:
5.4.3.1  0.3g.
5.4.4        Method of analysis:
5.4.4.1  Sample titration:
5.4.4.1.1        Take a flask and add in it 0.3g of sample.
5.4.4.1.2        Dissolve it in 50.0ml of a mixture of 1 volume of anhydrous acetic acid and 7 volumes of Methyl ethyl ketone.
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-3.
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 a mixture of 1 volume of anhydrous acetic acid and 7 volumes of Methyl ethyl ketone.
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-3.
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 42.59mg of Domperidone C22H24ClN5O2.
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: 2015, pp. 802-804.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Observations of Percentage Loss of drying by using oven.
Annexure 3: Observations and calculations of assay.

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 of percentage loss of drying
Percentage loss of drying
Weight of granules (Sample) = _____________
Time period = _____________
Sr.#
Time (min)
% Loss of Moisture


















Average % Loss of Moisture: _____________









% Loss of Moisture:

Optimum time for drying:





Annexure: 3
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
Ti
Initial temperature
Tf
Final temperature
Temp.
Temperature


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