OMEPRAZOLE SOP


OMEPRAZOLE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Omeprazole 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 (5 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        Dilute solutions of alkali hydroxides (e.g. dil. NaOH).
5.1.2.1.6        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 5 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 Methylene chloride 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.
5.1.2.3.6        Add dil. NaOH in test tube 5 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 Methylene chloride is soluble.
5.1.2.4.3        The sample in test tube 3 & 4 containing with Ethanol (96%) and methanol is sparingly soluble.
5.1.2.4.4        The sample in test tube 5 containing with dil. NaOH is dissolve.
5.2  Loss on drying:
5.2.1        Material and equipment:
5.2.1.1  Glassware (according to requirement).
5.2.1.2  Desiccator.
5.2.1.3  Diphosphorous pentaoxide (desiccant).
5.2.1.4  Analytical weighing balance.
5.2.1.5  Spatula.
5.2.2        Sample:
5.2.2.1  1.0g.
5.2.3        Method:
5.2.3.1  Weigh 1g of the test sample.
5.2.3.2  Set the desiccator apparatus with desiccant.
5.2.3.3  Operate the desiccator according to the SOP.
5.2.3.4  Place the sample into the china dish or petri dish.
5.2.3.5  Set the temperature 60oC and at 0.1kPa pressure for at least 4h.
5.2.3.6  And wait till the sample loses its moisture.
5.2.3.7  After 4h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.2.3.8  Note down readings on given Annexure-1.
5.2.4        Observations:
5.2.4.1  Maximum 0.5%.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Potentiometer.
5.3.1.3  Magnetic stirrer.
5.3.2        Material and reagents:
5.3.2.1  10.0ml of purified water.
5.3.2.2  40.0ml of ethanol (96%).
5.3.2.3  0.1M sodium hydroxide.
5.3.2.4  Thymolphthalein solution (as indicator).
5.3.3        Sample:
5.3.3.1  0.250g.
5.3.4        Method of analysis:
5.3.4.1  Take a 100.0ml of beaker and take 0.250g of sample in it.
5.3.4.2  Add a mixture of 10.0ml of purified water and 40.0ml of ethanol (96%) dissolve by using magnetic stirrer.
5.3.4.3  Fill the right hand side burette with titrant 0.1M sodium hydroxide.
5.3.4.4  Carry out a Potentiometric titration using thymolphthalein solution (as indicator).
5.3.4.5  Operate potentiometer according to SOP.
5.3.4.6  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.
5.3.4.7  Plot a graph, volume used v/s millivolts.
5.3.4.8  Find out the END POINT.
5.3.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.3.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-2.
5.3.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
Weight of sample
5.3.5        Factor:
5.3.5.1  1ml of 0.1M sodium hydroxide is equivalent to 34.54mg of Omeprazole C17H19N3O3S.
5.3.6        Limit:
5.3.6.1  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 / Omeprazole: 2015, pp. 439-441.
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
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: 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
Format
Q.C
Quality control
Vol
Volume
v/s
Verses
mV
Millivolts
g
Grams
ml
Milliliter
Min
Minutes
oC
Degree centigrade
mg
Milligram
M
Molar
%
Percentage
R
Reagent


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